# Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2000
# CCDC Number: 186/1746

data_global

#====================================================================

# 1. SUBMISSION DETAILS
_publ_contact_author  'Dr. Malcolm A. Halcrow'
_publ_contact_address
;
   School of Chemistry, 
   University of Leeds,
   Woodhouse Lane,
   Leeds LS2 9JT,
   UK
;
_publ_contact_author_phone       '+44 (0)113 2336506'
_publ_contact_author_fax         '+44 (0)113 2336565'
_publ_contact_author_email       malcolmh@chem.leeds.ac.uk
_publ_requested_journal          'Dalton Transactions'
_publ_contact_letter
;
The following set of data is for the complexes included in a Dalton full 
paper manuscript we have just submitted to you. 
;

#=======================================================================

# 2. TITLE AND AUTHOR LIST
_publ_section_title
;
 Steric Control of the Reactivity of Moderately Hindered Tris-
 pyrazolylborates with Copper(II) Salts.
;
loop_
_publ_author_name
   'Li Mei Lindy Chia'
   'Sanja Radojevic'
   'Ian J. Scowen'
   'Mary McPartlin'
   'Malcolm A. Halcrow'

_publ_author_address
;      
LMLC:
   Department of Chemistry, 
   University of Cambridge,
   Lensfield Road,
   Cambridge CB2 1EW,
   UK
SR, IJS & MMcP:
   School of Applied Chemistry, 
   University of North London,
   166-220 Holloway Road,
   London N7 8DB,
   UK
IJS:
   Department of Chemical and Forensic Sciences, 
   University of Bradford,
   Bradford BD7 1DP,
   UK
MAH:
   School of Chemistry, 
   University of Leeds,
   Woodhouse Lane,
   Leeds LS2 9JT,
   UK
;

#=================================================================
 
data_si267/mh312 
  
_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
Acetato[5-phenylpyrazole][hydrido-tris-{3-pyrazol-1-yl}borato]copper(II)
; 
_chemical_name_common             ?
_chemical_formula_sum             'C38 H33 B Cu N8 O2' 
_chemical_formula_weight          708.07 
  
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0033   0.0016 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'B'  'B'   0.0013   0.0007 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'N'  'N'   0.0061   0.0033 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'   0.0106   0.0060 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Cu'  'Cu'   0.3201   1.2651 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
  
_symmetry_cell_setting            Triclinic 
_symmetry_space_group_name_H-M    P-1 
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, -y, -z' 
  
_cell_length_a                    11.585(2) 
_cell_length_b                    16.787(4) 
_cell_length_c                    18.492(3) 
_cell_angle_alpha                 95.11(2) 
_cell_angle_beta                  106.077(13) 
_cell_angle_gamma                 94.17(3) 
_cell_volume                      3423.8(11) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     223(2) 
_cell_measurement_reflns_used     41 
_cell_measurement_theta_min       5.15 
_cell_measurement_theta_max       12.49 
  
_exptl_crystal_description        block 
_exptl_crystal_colour             green 
_exptl_crystal_size_max           0.40 
_exptl_crystal_size_mid           0.36 
_exptl_crystal_size_min           0.36 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.374 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              1468 
_exptl_absorpt_coefficient_mu     0.685 
_exptl_absorpt_correction_type    empirical 
_exptl_absorpt_correction_T_min   0.6913 
_exptl_absorpt_correction_T_max   0.8659 
  
_exptl_special_details 
; 
Crystal mounted under polybutene oil in liq. N2 cryostream
; 
  
_diffrn_ambient_temperature       223(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device        'Siemens P4' 
_diffrn_measurement_method        '2\q/\w scans' 
_diffrn_standards_number          3 
_diffrn_standards_interval_count  97 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         0
_diffrn_reflns_number             13981 
_diffrn_reflns_av_R_equivalents   0.0388 
_diffrn_reflns_av_sigmaI/netI     0.1196 
_diffrn_reflns_limit_h_min        -1 
_diffrn_reflns_limit_h_max        13 
_diffrn_reflns_limit_k_min        -19 
_diffrn_reflns_limit_k_max        19 
_diffrn_reflns_limit_l_min        -21 
_diffrn_reflns_limit_l_max        21 
_diffrn_reflns_theta_min          1.78 
_diffrn_reflns_theta_max          25.00 
_reflns_number_total              12026 
_reflns_number_observed           5529 
_reflns_observed_criterion        >2sigma(I) 
  
_computing_data_collection        'Siemens XSCANS' 
_computing_cell_refinement        'Siemens XSCANS' 
_computing_data_reduction         'Siemens SHELXTL' 
_computing_structure_solution     'SHELXS-86 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)' 
_computing_molecular_graphics     'Siemens SHELXTL' 
_computing_publication_material   'Siemens SHELXTL' 
  
_refine_special_details 
; 
 Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ 
 or flagged by the user for potential systematic errors.  Weighted R-factors 
 wR and all goodnesses of fit S are based on F^2^, conventional R-factors R 
 are based on F, with F set to zero for negative F^2^. The observed criterion 
 of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F^2^ are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
; 
  
_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme 
 'calc w=1/[\s^2^(Fo^2^)+(0.0552P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      none 
_refine_ls_number_reflns          12025 
_refine_ls_number_parameters      904 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.1425 
_refine_ls_R_factor_obs           0.0540 
_refine_ls_wR_factor_all          0.1571 
_refine_ls_wR_factor_obs          0.1088 
_refine_ls_goodness_of_fit_all    0.980 
_refine_ls_goodness_of_fit_obs    1.046 
_refine_ls_restrained_S_all       0.980 
_refine_ls_restrained_S_obs       1.046 
_refine_ls_shift/esd_max          0.036 
_refine_ls_shift/esd_mean         0.005 
  
loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_thermal_displace_type 
 _atom_site_occupancy 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_group 
Cu1 Cu -0.19642(6) 0.53722(4) 0.28085(4) 0.0326(2) Uani 1 d . . 
N11 N -0.3527(4) 0.6779(3) 0.2512(3) 0.0409(12) Uani 1 d . . 
N12 N -0.2925(4) 0.6303(2) 0.2127(3) 0.0356(11) Uani 1 d . . 
C11 C -0.4255(6) 0.7207(3) 0.2038(4) 0.054(2) Uani 1 d . . 
H11 H -0.4751(6) 0.7577(3) 0.2174(4) 0.065 Uiso 1 calc R . 
C12 C -0.4159(6) 0.7021(4) 0.1326(4) 0.061(2) Uani 1 d . . 
H12 H -0.4568(6) 0.7229(4) 0.0881(4) 0.073 Uiso 1 calc R . 
C13 C -0.3311(5) 0.6448(3) 0.1402(3) 0.0399(14) Uani 1 d . . 
C14 C -0.2784(5) 0.6101(3) 0.0825(3) 0.0398(15) Uani 1 d . . 
C15 C -0.1538(5) 0.6082(3) 0.0974(3) 0.043(2) Uani 1 d . . 
H15 H -0.1032(5) 0.6261(3) 0.1463(3) 0.052 Uiso 1 calc R . 
C16 C -0.1040(6) 0.5808(3) 0.0419(4) 0.049(2) Uani 1 d . . 
H16 H -0.0199(6) 0.5797(3) 0.0530(4) 0.059 Uiso 1 calc R . 
C17 C -0.1769(6) 0.5549(4) -0.0300(4) 0.056(2) Uani 1 d . . 
H17 H -0.1421(6) 0.5371(4) -0.0680(4) 0.067 Uiso 1 calc R . 
C18 C -0.2995(7) 0.5548(4) -0.0467(4) 0.064(2) Uani 1 d . . 
H18 H -0.3494(7) 0.5361(4) -0.0956(4) 0.077 Uiso 1 calc R . 
C19 C -0.3492(6) 0.5829(4) 0.0101(4) 0.055(2) Uani 1 d . . 
H19 H -0.4335(6) 0.5833(4) -0.0013(4) 0.066 Uiso 1 calc R . 
N21 N -0.2057(4) 0.6776(3) 0.3801(3) 0.0414(12) Uani 1 d . . 
N22 N -0.1288(4) 0.6212(2) 0.3710(3) 0.0351(11) Uani 1 d . . 
C21 C -0.1448(6) 0.7369(3) 0.4325(4) 0.055(2) Uani 1 d . . 
H21 H -0.1773(6) 0.7826(3) 0.4486(4) 0.067 Uiso 1 calc R . 
C22 C -0.0277(6) 0.7207(3) 0.4593(3) 0.050(2) Uani 1 d . . 
H22 H 0.0348(6) 0.7523(3) 0.4966(3) 0.060 Uiso 1 calc R . 
C23 C -0.0198(5) 0.6475(3) 0.4198(3) 0.0373(14) Uani 1 d . . 
C24 C 0.0842(5) 0.5997(3) 0.4326(3) 0.0352(14) Uani 1 d . . 
C25 C 0.0674(5) 0.5162(3) 0.4314(3) 0.0409(15) Uani 1 d . . 
H25 H -0.0111(5) 0.4898(3) 0.4185(3) 0.049 Uiso 1 calc R . 
C26 C 0.1658(6) 0.4726(4) 0.4490(3) 0.051(2) Uani 1 d . . 
H26 H 0.1537(6) 0.4163(4) 0.4466(3) 0.061 Uiso 1 calc R . 
C27 C 0.2816(6) 0.5104(4) 0.4700(3) 0.054(2) Uani 1 d . . 
H27 H 0.3484(6) 0.4806(4) 0.4833(3) 0.065 Uiso 1 calc R . 
C28 C 0.2978(6) 0.5924(4) 0.4712(3) 0.051(2) Uani 1 d . . 
H28 H 0.3765(6) 0.6186(4) 0.4846(3) 0.061 Uiso 1 calc R . 
C29 C 0.2008(5) 0.6371(4) 0.4532(3) 0.047(2) Uani 1 d . . 
H29 H 0.2139(5) 0.6932(4) 0.4548(3) 0.056 Uiso 1 calc R . 
N31 N -0.3939(4) 0.5839(3) 0.3400(3) 0.0404(12) Uani 1 d . . 
N32 N -0.3365(4) 0.5178(3) 0.3268(2) 0.0352(11) Uani 1 d . . 
C31 C -0.4993(5) 0.5587(4) 0.3528(3) 0.048(2) Uani 1 d . . 
H31 H -0.5559(5) 0.5923(4) 0.3627(3) 0.057 Uiso 1 calc R . 
C32 C -0.5105(5) 0.4770(4) 0.3488(3) 0.049(2) Uani 1 d . . 
H32 H -0.5751(5) 0.4439(4) 0.3551(3) 0.059 Uiso 1 calc R . 
C33 C -0.4061(5) 0.4524(3) 0.3335(3) 0.0383(14) Uani 1 d . . 
C34 C -0.3656(5) 0.3722(3) 0.3300(3) 0.0364(14) Uani 1 d . . 
C35 C -0.4471(6) 0.3036(3) 0.3016(3) 0.047(2) Uani 1 d . . 
H35 H -0.5302(6) 0.3084(3) 0.2835(3) 0.057 Uiso 1 calc R . 
C36 C -0.4046(7) 0.2287(4) 0.3003(4) 0.063(2) Uani 1 d . . 
H36 H -0.4601(7) 0.1827(4) 0.2822(4) 0.075 Uiso 1 calc R . 
C37 C -0.2851(7) 0.2199(4) 0.3246(4) 0.058(2) Uani 1 d . . 
H37 H -0.2574(7) 0.1688(4) 0.3216(4) 0.070 Uiso 1 calc R . 
C38 C -0.2058(6) 0.2869(4) 0.3533(3) 0.050(2) Uani 1 d . . 
H38 H -0.1230(6) 0.2812(4) 0.3716(3) 0.060 Uiso 1 calc R . 
C39 C -0.2442(5) 0.3623(3) 0.3563(3) 0.0411(15) Uani 1 d . . 
H39 H -0.1876(5) 0.4074(3) 0.3763(3) 0.049 Uiso 1 calc R . 
B1 B -0.3403(6) 0.6682(4) 0.3347(4) 0.045(2) Uani 1 d . . 
H1 H -0.3833(6) 0.7090(4) 0.3559(4) 0.054 Uiso 1 calc R . 
N41 N -0.2698(4) 0.4476(2) 0.2004(2) 0.0345(11) Uani 1 d . . 
N42 N -0.2138(4) 0.3801(2) 0.1940(2) 0.0333(11) Uani 1 d . . 
H42N H -0.1166 0.3796 0.2102 0.099(19) Uiso 1 d . . 
C41 C -0.3825(5) 0.4283(3) 0.1594(3) 0.0389(14) Uani 1 d . . 
H41 H -0.4423(5) 0.4641(3) 0.1524(3) 0.047 Uiso 1 calc R . 
C42 C -0.4026(5) 0.3484(3) 0.1275(3) 0.043(2) Uani 1 d . . 
H42 H -0.4757(5) 0.3205(3) 0.0972(3) 0.052 Uiso 1 calc R . 
C43 C -0.2917(5) 0.3192(3) 0.1503(3) 0.0338(13) Uani 1 d . . 
C44 C -0.2534(5) 0.2390(3) 0.1361(3) 0.0392(14) Uani 1 d . . 
C45 C -0.1487(6) 0.2152(3) 0.1826(3) 0.046(2) Uani 1 d . . 
H45 H -0.1018(6) 0.2507(3) 0.2243(3) 0.056 Uiso 1 calc R . 
C46 C -0.1120(6) 0.1401(4) 0.1685(4) 0.059(2) Uani 1 d . . 
H46 H -0.0411(6) 0.1244(4) 0.2005(4) 0.071 Uiso 1 calc R . 
C47 C -0.1816(7) 0.0879(4) 0.1063(5) 0.065(2) Uani 1 d . . 
H47 H -0.1582(7) 0.0366(4) 0.0962(5) 0.079 Uiso 1 calc R . 
C48 C -0.2837(7) 0.1118(4) 0.0601(5) 0.076(2) Uani 1 d . . 
H48 H -0.3299(7) 0.0769(4) 0.0177(5) 0.091 Uiso 1 calc R . 
C49 C -0.3203(6) 0.1871(3) 0.0750(4) 0.056(2) Uani 1 d . . 
H49 H -0.3913(6) 0.2025(3) 0.0430(4) 0.067 Uiso 1 calc R . 
O51 O -0.0399(3) 0.5466(2) 0.2597(2) 0.0333(9) Uani 1 d . . 
C51 C 0.0338(5) 0.4957(4) 0.2549(3) 0.042(2) Uani 1 d . . 
O52 O 0.0159(4) 0.4223(2) 0.2588(3) 0.0646(14) Uani 1 d . . 
C52 C 0.1527(5) 0.5289(4) 0.2469(4) 0.057(2) Uani 1 d . . 
H52A H 0.1967(15) 0.5635(19) 0.2925(9) 0.085 Uiso 1 calc R . 
H52B H 0.1390(5) 0.5597(19) 0.2038(13) 0.085 Uiso 1 calc R . 
H52C H 0.1995(15) 0.4850(4) 0.2390(22) 0.085 Uiso 1 calc R . 
Cu2 Cu 0.31282(6) 1.05504(4) 0.28481(4) 0.0317(2) Uani 1 d . . 
N61 N 0.2291(4) 1.2259(2) 0.2775(2) 0.0346(11) Uani 1 d . . 
N62 N 0.2690(4) 1.1744(2) 0.2305(3) 0.0344(11) Uani 1 d . . 
C61 C 0.1952(5) 1.2917(3) 0.2442(4) 0.045(2) Uani 1 d . . 
H61 H 0.1640(5) 1.3352(3) 0.2655(4) 0.054 Uiso 1 calc R . 
C62 C 0.2135(5) 1.2850(3) 0.1745(4) 0.048(2) Uani 1 d . . 
H62 H 0.1984(5) 1.3222(3) 0.1387(4) 0.057 Uiso 1 calc R . 
C63 C 0.2599(5) 1.2107(3) 0.1673(3) 0.0357(14) Uani 1 d . . 
C64 C 0.2932(5) 1.1750(3) 0.1017(3) 0.0365(14) Uani 1 d . . 
C65 C 0.3723(5) 1.1153(3) 0.1073(3) 0.0418(15) Uani 1 d . . 
H65 H 0.4058(5) 1.0969(3) 0.1544(3) 0.050 Uiso 1 calc R . 
C66 C 0.4012(6) 1.0834(3) 0.0441(4) 0.050(2) Uani 1 d . . 
H66 H 0.4548(6) 1.0434(3) 0.0487(4) 0.060 Uiso 1 calc R . 
C67 C 0.3537(7) 1.1085(4) -0.0247(4) 0.063(2) Uani 1 d . . 
H67 H 0.3736(7) 1.0854(4) -0.0673(4) 0.075 Uiso 1 calc R . 
C68 C 0.2766(7) 1.1677(4) -0.0322(4) 0.063(2) Uani 1 d . . 
H68 H 0.2442(7) 1.1856(4) -0.0797(4) 0.075 Uiso 1 calc R . 
C69 C 0.2468(6) 1.2011(4) 0.0312(4) 0.053(2) Uani 1 d . . 
H69 H 0.1945(6) 1.2418(4) 0.0261(4) 0.064 Uiso 1 calc R . 
N71 N 0.3514(4) 1.1896(2) 0.4027(3) 0.0356(11) Uani 1 d . . 
N72 N 0.4054(4) 1.1234(2) 0.3846(2) 0.0300(10) Uani 1 d . . 
C71 C 0.4242(5) 1.2345(3) 0.4633(3) 0.044(2) Uani 1 d . . 
H71 H 0.4068(5) 1.2831(3) 0.4854(3) 0.053 Uiso 1 calc R . 
C72 C 0.5281(5) 1.1991(3) 0.4884(3) 0.0415(15) Uani 1 d . . 
H72 H 0.5945(5) 1.2175(3) 0.5305(3) 0.050 Uiso 1 calc R . 
C73 C 0.5141(5) 1.1292(3) 0.4376(3) 0.0342(13) Uani 1 d . . 
C74 C 0.6022(5) 1.0703(3) 0.4441(3) 0.0317(13) Uani 1 d . . 
C75 C 0.5689(5) 0.9877(3) 0.4291(3) 0.0405(15) Uani 1 d . . 
H75 H 0.4869(5) 0.9680(3) 0.4112(3) 0.049 Uiso 1 calc R . 
C76 C 0.6566(6) 0.9349(3) 0.4407(3) 0.046(2) Uani 1 d . . 
H76 H 0.6333(6) 0.8793(3) 0.4294(3) 0.056 Uiso 1 calc R . 
C77 C 0.7781(6) 0.9621(4) 0.4686(3) 0.048(2) Uani 1 d . . 
H77 H 0.8369(6) 0.9255(4) 0.4765(3) 0.058 Uiso 1 calc R . 
C78 C 0.8114(5) 1.0434(4) 0.4847(3) 0.046(2) Uani 1 d . . 
H78 H 0.8934(5) 1.0628(4) 0.5047(3) 0.055 Uiso 1 calc R . 
C79 C 0.7251(5) 1.0964(3) 0.4715(3) 0.0413(15) Uani 1 d . . 
H79 H 0.7495(5) 1.1518(3) 0.4812(3) 0.050 Uiso 1 calc R . 
N81 N 0.1394(4) 1.1297(2) 0.3493(2) 0.0347(11) Uani 1 d . . 
N82 N 0.1661(4) 1.0560(2) 0.3229(2) 0.0318(11) Uani 1 d . . 
C81 C 0.0334(5) 1.1215(3) 0.3654(3) 0.0409(15) Uani 1 d . . 
H81 H -0.0045(5) 1.1633(3) 0.3837(3) 0.049 Uiso 1 calc R . 
C82 C -0.0103(5) 1.0418(3) 0.3505(3) 0.0392(14) Uani 1 d . . 
H82 H -0.0832(5) 1.0186(3) 0.3561(3) 0.047 Uiso 1 calc R . 
C83 C 0.0755(5) 1.0020(3) 0.3254(3) 0.0332(13) Uani 1 d . . 
C84 C 0.0753(5) 0.9156(3) 0.3072(3) 0.0352(14) Uani 1 d . . 
C85 C -0.0345(6) 0.8690(4) 0.2753(4) 0.058(2) Uani 1 d . . 
H85 H -0.1064(6) 0.8939(4) 0.2629(4) 0.070 Uiso 1 calc R . 
C86 C -0.0389(7) 0.7866(4) 0.2615(4) 0.075(2) Uani 1 d . . 
H86 H -0.1136(7) 0.7555(4) 0.2408(4) 0.090 Uiso 1 calc R . 
C87 C 0.0659(8) 0.7500(4) 0.2781(4) 0.069(2) Uani 1 d . . 
H87 H 0.0629(8) 0.6938(4) 0.2688(4) 0.082 Uiso 1 calc R . 
C88 C 0.1751(7) 0.7950(4) 0.3082(4) 0.056(2) Uani 1 d . . 
H88 H 0.2468(7) 0.7698(4) 0.3185(4) 0.067 Uiso 1 calc R . 
C89 C 0.1799(6) 0.8777(3) 0.3234(3) 0.043(2) Uani 1 d . . 
H89 H 0.2549(6) 0.9083(3) 0.3449(3) 0.051 Uiso 1 calc R . 
B2 B 0.2249(6) 1.2051(4) 0.3552(4) 0.040(2) Uani 1 d . . 
H2 H 0.1972(6) 1.2507(4) 0.3815(4) 0.048 Uiso 1 calc R . 
N91 N 0.2138(4) 0.9886(2) 0.1904(2) 0.0326(11) Uani 1 d . . 
N92 N 0.2359(4) 0.9137(2) 0.1676(3) 0.0362(11) Uani 1 d . . 
H92N H 0.3044 0.8964 0.2022 0.099(19) Uiso 1 d . . 
C91 C 0.1120(5) 1.0015(3) 0.1396(3) 0.043(2) Uani 1 d . . 
H91 H 0.0748(5) 1.0494(3) 0.1398(3) 0.051 Uiso 1 calc R . 
C92 C 0.0686(5) 0.9347(3) 0.0864(3) 0.044(2) Uani 1 d . . 
H92 H -0.0020(5) 0.9287(3) 0.0455(3) 0.053 Uiso 1 calc R . 
C93 C 0.1499(5) 0.8794(3) 0.1056(3) 0.0370(14) Uani 1 d . . 
C94 C 0.1559(5) 0.7981(3) 0.0705(3) 0.0386(14) Uani 1 d . . 
C95 C 0.0793(5) 0.7703(3) -0.0003(3) 0.044(2) Uani 1 d . . 
H95 H 0.0205(5) 0.8023(3) -0.0247(3) 0.052 Uiso 1 calc R . 
C96 C 0.0883(6) 0.6954(3) -0.0358(3) 0.049(2) Uani 1 d . . 
H96 H 0.0352(6) 0.6772(3) -0.0839(3) 0.059 Uiso 1 calc R . 
C97 C 0.1736(6) 0.6479(3) -0.0014(4) 0.051(2) Uani 1 d . . 
H97 H 0.1807(6) 0.5978(3) -0.0258(4) 0.062 Uiso 1 calc R . 
C98 C 0.2488(6) 0.6750(4) 0.0696(4) 0.059(2) Uani 1 d . . 
H98 H 0.3066(6) 0.6424(4) 0.0941(4) 0.071 Uiso 1 calc R . 
C99 C 0.2411(6) 0.7489(3) 0.1056(4) 0.053(2) Uani 1 d . . 
H99 H 0.2936(6) 0.7663(3) 0.1540(4) 0.063 Uiso 1 calc R . 
O53 O 0.4641(3) 1.0336(2) 0.2658(2) 0.0337(9) Uani 1 d . . 
C53 C 0.5088(5) 0.9673(4) 0.2564(3) 0.0394(15) Uani 1 d . . 
O54 O 0.4564(4) 0.8993(2) 0.2536(2) 0.0525(12) Uani 1 d . . 
C54 C 0.6352(5) 0.9756(4) 0.2491(4) 0.063(2) Uani 1 d . . 
H54A H 0.6909(7) 0.9983(23) 0.2973(7) 0.095 Uiso 1 calc R . 
H54B H 0.6392(10) 1.0108(20) 0.2108(16) 0.095 Uiso 1 calc R . 
H54C H 0.6570(14) 0.9232(5) 0.2344(23) 0.095 Uiso 1 calc R . 
  
loop_ 
 _atom_site_aniso_label 
 _atom_site_aniso_U_11 
 _atom_site_aniso_U_22 
 _atom_site_aniso_U_33 
 _atom_site_aniso_U_23 
 _atom_site_aniso_U_13 
 _atom_site_aniso_U_12 
Cu1 0.0271(4) 0.0316(4) 0.0407(4) 0.0012(3) 0.0113(3) 0.0110(3) 
N11 0.036(3) 0.033(3) 0.059(3) 0.008(2) 0.020(3) 0.018(2) 
N12 0.034(3) 0.031(2) 0.045(3) 0.007(2) 0.013(2) 0.017(2) 
C11 0.044(4) 0.049(4) 0.080(5) 0.027(4) 0.021(4) 0.030(3) 
C12 0.052(5) 0.073(5) 0.068(5) 0.033(4) 0.020(4) 0.034(4) 
C13 0.026(3) 0.043(3) 0.052(4) 0.017(3) 0.009(3) 0.009(3) 
C14 0.045(4) 0.037(3) 0.041(4) 0.020(3) 0.012(3) 0.007(3) 
C15 0.034(4) 0.052(4) 0.047(4) 0.012(3) 0.013(3) 0.011(3) 
C16 0.043(4) 0.058(4) 0.058(4) 0.024(3) 0.024(4) 0.017(3) 
C17 0.067(5) 0.060(4) 0.049(4) 0.018(3) 0.019(4) 0.022(4) 
C18 0.060(5) 0.078(5) 0.046(4) 0.012(4) -0.001(4) 0.017(4) 
C19 0.042(4) 0.060(4) 0.060(5) 0.014(4) 0.004(4) 0.013(3) 
N21 0.038(3) 0.033(3) 0.052(3) -0.006(2) 0.012(3) 0.011(2) 
N22 0.032(3) 0.033(3) 0.045(3) -0.001(2) 0.020(2) 0.009(2) 
C21 0.049(4) 0.040(4) 0.068(5) -0.016(3) 0.008(4) 0.011(3) 
C22 0.053(4) 0.033(3) 0.054(4) -0.014(3) 0.007(4) 0.000(3) 
C23 0.038(4) 0.036(3) 0.041(3) -0.002(3) 0.018(3) 0.005(3) 
C24 0.032(3) 0.040(3) 0.038(3) 0.005(3) 0.016(3) 0.008(3) 
C25 0.030(3) 0.048(4) 0.043(4) 0.004(3) 0.008(3) 0.006(3) 
C26 0.050(4) 0.049(4) 0.054(4) 0.007(3) 0.014(4) 0.012(3) 
C27 0.043(4) 0.072(5) 0.048(4) 0.005(3) 0.010(3) 0.034(4) 
C28 0.032(4) 0.073(5) 0.047(4) -0.006(3) 0.013(3) 0.007(3) 
C29 0.036(4) 0.046(4) 0.056(4) -0.005(3) 0.015(3) -0.003(3) 
N31 0.037(3) 0.044(3) 0.044(3) 0.000(2) 0.016(3) 0.019(2) 
N32 0.031(3) 0.035(3) 0.041(3) 0.002(2) 0.012(2) 0.009(2) 
C31 0.023(3) 0.071(5) 0.057(4) 0.008(3) 0.020(3) 0.015(3) 
C32 0.035(4) 0.061(4) 0.058(4) 0.017(3) 0.020(3) 0.010(3) 
C33 0.026(3) 0.048(4) 0.040(3) 0.006(3) 0.009(3) 0.003(3) 
C34 0.035(4) 0.038(3) 0.033(3) 0.007(3) 0.004(3) 0.004(3) 
C35 0.042(4) 0.052(4) 0.049(4) 0.008(3) 0.016(3) -0.005(3) 
C36 0.084(6) 0.037(4) 0.071(5) 0.008(3) 0.035(5) -0.016(4) 
C37 0.082(6) 0.037(4) 0.066(5) 0.014(3) 0.035(5) 0.012(4) 
C38 0.053(4) 0.052(4) 0.051(4) 0.015(3) 0.020(4) 0.015(4) 
C39 0.037(4) 0.037(3) 0.049(4) 0.008(3) 0.010(3) 0.001(3) 
B1 0.044(5) 0.035(4) 0.059(5) -0.002(3) 0.019(4) 0.022(3) 
N41 0.030(3) 0.033(3) 0.041(3) 0.004(2) 0.011(2) 0.012(2) 
N42 0.031(3) 0.029(2) 0.042(3) 0.003(2) 0.014(2) 0.010(2) 
C41 0.032(4) 0.038(3) 0.045(4) 0.012(3) 0.005(3) 0.014(3) 
C42 0.035(4) 0.033(3) 0.049(4) 0.000(3) -0.006(3) -0.001(3) 
C43 0.032(3) 0.039(3) 0.032(3) 0.005(3) 0.012(3) 0.002(3) 
C44 0.040(4) 0.033(3) 0.048(4) 0.002(3) 0.019(3) 0.006(3) 
C45 0.053(4) 0.044(4) 0.044(4) 0.001(3) 0.015(3) 0.015(3) 
C46 0.069(5) 0.050(4) 0.066(5) 0.009(4) 0.025(4) 0.024(4) 
C47 0.065(5) 0.036(4) 0.106(6) 0.007(4) 0.040(5) 0.011(4) 
C48 0.062(5) 0.042(4) 0.116(7) -0.022(4) 0.027(5) -0.004(4) 
C49 0.034(4) 0.044(4) 0.081(5) -0.009(4) 0.008(4) -0.003(3) 
O51 0.026(2) 0.034(2) 0.046(2) 0.003(2) 0.017(2) 0.015(2) 
C51 0.031(4) 0.048(4) 0.044(4) -0.004(3) 0.006(3) 0.009(3) 
O52 0.032(3) 0.037(2) 0.112(4) -0.005(2) 0.001(3) 0.014(2) 
C52 0.036(4) 0.064(4) 0.075(5) -0.007(4) 0.026(4) 0.009(3) 
Cu2 0.0270(4) 0.0292(4) 0.0416(4) 0.0011(3) 0.0136(3) 0.0086(3) 
N61 0.036(3) 0.025(2) 0.048(3) 0.008(2) 0.018(2) 0.014(2) 
N62 0.038(3) 0.023(2) 0.047(3) 0.006(2) 0.018(2) 0.010(2) 
C61 0.043(4) 0.031(3) 0.066(4) 0.013(3) 0.018(3) 0.020(3) 
C62 0.051(4) 0.035(3) 0.063(4) 0.021(3) 0.018(4) 0.017(3) 
C63 0.030(3) 0.030(3) 0.051(4) 0.012(3) 0.013(3) 0.010(3) 
C64 0.032(3) 0.032(3) 0.046(4) 0.011(3) 0.011(3) 0.000(3) 
C65 0.048(4) 0.041(3) 0.039(4) 0.008(3) 0.014(3) 0.010(3) 
C66 0.051(4) 0.047(4) 0.054(4) -0.002(3) 0.021(4) -0.001(3) 
C67 0.078(6) 0.065(5) 0.049(4) -0.006(4) 0.030(4) -0.003(4) 
C68 0.072(5) 0.070(5) 0.045(4) 0.013(4) 0.017(4) -0.007(4) 
C69 0.048(4) 0.055(4) 0.059(4) 0.019(3) 0.014(4) 0.006(3) 
N71 0.033(3) 0.021(2) 0.054(3) -0.002(2) 0.015(3) 0.005(2) 
N72 0.025(3) 0.025(2) 0.042(3) 0.002(2) 0.015(2) 0.004(2) 
C71 0.047(4) 0.029(3) 0.056(4) -0.007(3) 0.018(3) 0.000(3) 
C72 0.042(4) 0.040(3) 0.038(3) -0.005(3) 0.008(3) -0.002(3) 
C73 0.035(4) 0.029(3) 0.044(3) 0.002(3) 0.021(3) 0.001(3) 
C74 0.030(3) 0.036(3) 0.031(3) 0.004(2) 0.010(3) 0.003(3) 
C75 0.040(4) 0.036(3) 0.047(4) 0.009(3) 0.013(3) 0.010(3) 
C76 0.049(4) 0.042(4) 0.051(4) 0.012(3) 0.015(3) 0.009(3) 
C77 0.038(4) 0.059(4) 0.052(4) 0.016(3) 0.013(3) 0.026(3) 
C78 0.028(4) 0.063(4) 0.048(4) 0.010(3) 0.009(3) 0.014(3) 
C79 0.039(4) 0.043(3) 0.041(4) 0.006(3) 0.010(3) 0.002(3) 
N81 0.032(3) 0.033(3) 0.042(3) -0.001(2) 0.014(2) 0.012(2) 
N82 0.025(3) 0.025(2) 0.048(3) 0.002(2) 0.013(2) 0.008(2) 
C81 0.031(4) 0.050(4) 0.045(4) 0.002(3) 0.015(3) 0.011(3) 
C82 0.021(3) 0.054(4) 0.049(4) 0.004(3) 0.019(3) 0.008(3) 
C83 0.023(3) 0.041(3) 0.037(3) 0.006(3) 0.012(3) 0.002(3) 
C84 0.036(4) 0.028(3) 0.046(4) 0.006(3) 0.020(3) 0.001(3) 
C85 0.041(4) 0.052(4) 0.078(5) -0.003(4) 0.016(4) -0.008(3) 
C86 0.064(5) 0.054(5) 0.101(6) -0.014(4) 0.030(5) -0.032(4) 
C87 0.098(7) 0.036(4) 0.073(5) -0.005(4) 0.033(5) -0.009(4) 
C88 0.073(5) 0.044(4) 0.057(4) 0.014(3) 0.022(4) 0.016(4) 
C89 0.050(4) 0.031(3) 0.046(4) 0.004(3) 0.013(3) 0.004(3) 
B2 0.041(4) 0.025(3) 0.060(5) 0.000(3) 0.023(4) 0.010(3) 
N91 0.028(3) 0.030(2) 0.040(3) 0.000(2) 0.012(2) 0.005(2) 
N92 0.036(3) 0.032(3) 0.039(3) 0.001(2) 0.008(2) 0.011(2) 
C91 0.038(4) 0.042(3) 0.047(4) 0.000(3) 0.008(3) 0.019(3) 
C92 0.040(4) 0.037(3) 0.044(4) -0.008(3) -0.004(3) 0.009(3) 
C93 0.036(4) 0.038(3) 0.037(3) -0.001(3) 0.011(3) 0.007(3) 
C94 0.036(4) 0.036(3) 0.043(4) -0.001(3) 0.011(3) 0.004(3) 
C95 0.036(4) 0.046(4) 0.048(4) 0.001(3) 0.013(3) 0.002(3) 
C96 0.054(4) 0.045(4) 0.044(4) -0.008(3) 0.015(3) -0.013(3) 
C97 0.060(5) 0.036(3) 0.061(4) -0.004(3) 0.026(4) -0.002(3) 
C98 0.066(5) 0.041(4) 0.069(5) 0.003(3) 0.015(4) 0.022(4) 
C99 0.054(4) 0.036(3) 0.057(4) -0.006(3) -0.001(4) 0.010(3) 
O53 0.025(2) 0.030(2) 0.046(2) 0.002(2) 0.009(2) 0.010(2) 
C53 0.034(4) 0.050(4) 0.030(3) -0.006(3) 0.003(3) 0.012(3) 
O54 0.041(3) 0.030(2) 0.078(3) -0.002(2) 0.003(2) 0.017(2) 
C54 0.038(4) 0.076(5) 0.084(5) 0.003(4) 0.029(4) 0.021(4) 
  
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
  
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
Cu1 O51 1.957(3) . ? 
Cu1 N41 1.978(4) . ? 
Cu1 N22 2.020(4) . ? 
Cu1 N32 2.049(5) . ? 
Cu1 N12 2.257(4) . ? 
N11 C11 1.337(7) . ? 
N11 N12 1.373(6) . ? 
N11 B1 1.535(8) . ? 
N12 C13 1.341(7) . ? 
C11 C12 1.362(8) . ? 
C12 C13 1.413(7) . ? 
C13 C14 1.468(8) . ? 
C14 C19 1.379(8) . ? 
C14 C15 1.396(8) . ? 
C15 C16 1.371(8) . ? 
C16 C17 1.375(8) . ? 
C17 C18 1.367(9) . ? 
C18 C19 1.393(8) . ? 
N21 C21 1.332(7) . ? 
N21 N22 1.376(5) . ? 
N21 B1 1.542(8) . ? 
N22 C23 1.349(7) . ? 
C21 C22 1.366(8) . ? 
C22 C23 1.394(7) . ? 
C23 C24 1.473(7) . ? 
C24 C29 1.384(7) . ? 
C24 C25 1.397(7) . ? 
C25 C26 1.379(7) . ? 
C26 C27 1.378(8) . ? 
C27 C28 1.374(8) . ? 
C28 C29 1.376(8) . ? 
N31 C31 1.352(7) . ? 
N31 N32 1.371(5) . ? 
N31 B1 1.527(8) . ? 
N32 C33 1.349(7) . ? 
C31 C32 1.362(8) . ? 
C32 C33 1.398(7) . ? 
C33 C34 1.460(7) . ? 
C34 C39 1.383(7) . ? 
C34 C35 1.396(7) . ? 
C35 C36 1.384(8) . ? 
C36 C37 1.356(9) . ? 
C37 C38 1.364(8) . ? 
C38 C39 1.373(7) . ? 
N41 C41 1.316(6) . ? 
N41 N42 1.359(5) . ? 
N42 C43 1.352(6) . ? 
C41 C42 1.392(7) . ? 
C42 C43 1.378(7) . ? 
C43 C44 1.472(7) . ? 
C44 C49 1.370(8) . ? 
C44 C45 1.387(8) . ? 
C45 C46 1.386(7) . ? 
C46 C47 1.394(9) . ? 
C47 C48 1.364(9) . ? 
C48 C49 1.391(8) . ? 
O51 C51 1.266(6) . ? 
C51 O52 1.247(6) . ? 
C51 C52 1.499(8) . ? 
Cu2 O53 1.933(3) . ? 
Cu2 N91 1.992(4) . ? 
Cu2 N82 2.013(4) . ? 
Cu2 N72 2.054(4) . ? 
Cu2 N62 2.347(4) . ? 
N61 C61 1.343(6) . ? 
N61 N62 1.366(5) . ? 
N61 B2 1.522(8) . ? 
N62 C63 1.347(6) . ? 
C61 C62 1.359(8) . ? 
C62 C63 1.403(7) . ? 
C63 C64 1.463(7) . ? 
C64 C69 1.388(7) . ? 
C64 C65 1.398(7) . ? 
C65 C66 1.378(7) . ? 
C66 C67 1.357(8) . ? 
C67 C68 1.375(9) . ? 
C68 C69 1.393(8) . ? 
N71 C71 1.330(7) . ? 
N71 N72 1.374(5) . ? 
N71 B2 1.540(8) . ? 
N72 C73 1.356(6) . ? 
C71 C72 1.364(7) . ? 
C72 C73 1.407(7) . ? 
C73 C74 1.460(7) . ? 
C74 C75 1.393(7) . ? 
C74 C79 1.395(7) . ? 
C75 C76 1.382(7) . ? 
C76 C77 1.386(8) . ? 
C77 C78 1.374(8) . ? 
C78 C79 1.372(7) . ? 
N81 C81 1.342(7) . ? 
N81 N82 1.378(5) . ? 
N81 B2 1.526(7) . ? 
N82 C83 1.349(6) . ? 
C81 C82 1.372(7) . ? 
C82 C83 1.394(7) . ? 
C83 C84 1.460(7) . ? 
C84 C89 1.382(7) . ? 
C84 C85 1.391(8) . ? 
C85 C86 1.379(8) . ? 
C86 C87 1.372(9) . ? 
C87 C88 1.370(9) . ? 
C88 C89 1.386(7) . ? 
N91 C91 1.334(6) . ? 
N91 N92 1.354(5) . ? 
N92 C93 1.343(6) . ? 
C91 C92 1.388(7) . ? 
C92 C93 1.369(7) . ? 
C93 C94 1.473(7) . ? 
C94 C95 1.380(7) . ? 
C94 C99 1.392(7) . ? 
C95 C96 1.389(7) . ? 
C96 C97 1.369(8) . ? 
C97 C98 1.376(8) . ? 
C98 C99 1.375(7) . ? 
O53 C53 1.279(6) . ? 
C53 O54 1.244(6) . ? 
C53 C54 1.505(8) . ? 
  
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
O51 Cu1 N41 95.4(2) . . ? 
O51 Cu1 N22 89.0(2) . . ? 
N41 Cu1 N22 173.4(2) . . ? 
O51 Cu1 N32 166.1(2) . . ? 
N41 Cu1 N32 89.8(2) . . ? 
N22 Cu1 N32 84.8(2) . . ? 
O51 Cu1 N12 101.6(2) . . ? 
N41 Cu1 N12 93.5(2) . . ? 
N22 Cu1 N12 90.4(2) . . ? 
N32 Cu1 N12 90.9(2) . . ? 
C11 N11 N12 110.3(5) . . ? 
C11 N11 B1 130.2(5) . . ? 
N12 N11 B1 119.0(4) . . ? 
C13 N12 N11 105.8(4) . . ? 
C13 N12 Cu1 138.9(4) . . ? 
N11 N12 Cu1 113.6(3) . . ? 
N11 C11 C12 108.9(5) . . ? 
C11 C12 C13 105.0(6) . . ? 
N12 C13 C12 110.0(5) . . ? 
N12 C13 C14 121.7(5) . . ? 
C12 C13 C14 128.0(6) . . ? 
C19 C14 C15 117.4(6) . . ? 
C19 C14 C13 121.3(6) . . ? 
C15 C14 C13 121.1(6) . . ? 
C16 C15 C14 121.1(6) . . ? 
C15 C16 C17 120.1(6) . . ? 
C18 C17 C16 120.6(7) . . ? 
C17 C18 C19 118.8(6) . . ? 
C14 C19 C18 121.9(6) . . ? 
C21 N21 N22 109.2(5) . . ? 
C21 N21 B1 128.5(5) . . ? 
N22 N21 B1 122.3(4) . . ? 
C23 N22 N21 106.7(4) . . ? 
C23 N22 Cu1 137.3(4) . . ? 
N21 N22 Cu1 114.9(3) . . ? 
N21 C21 C22 109.3(5) . . ? 
C21 C22 C23 105.8(5) . . ? 
N22 C23 C22 109.1(5) . . ? 
N22 C23 C24 123.2(5) . . ? 
C22 C23 C24 127.4(6) . . ? 
C29 C24 C25 118.6(5) . . ? 
C29 C24 C23 120.6(5) . . ? 
C25 C24 C23 120.5(5) . . ? 
C26 C25 C24 120.1(6) . . ? 
C27 C26 C25 120.8(6) . . ? 
C28 C27 C26 118.9(6) . . ? 
C27 C28 C29 121.2(6) . . ? 
C28 C29 C24 120.3(6) . . ? 
C31 N31 N32 108.6(5) . . ? 
C31 N31 B1 130.6(5) . . ? 
N32 N31 B1 120.8(5) . . ? 
C33 N32 N31 107.3(5) . . ? 
C33 N32 Cu1 135.0(4) . . ? 
N31 N32 Cu1 115.9(3) . . ? 
N31 C31 C32 109.1(5) . . ? 
C31 C32 C33 106.0(5) . . ? 
N32 C33 C32 109.0(5) . . ? 
N32 C33 C34 121.5(5) . . ? 
C32 C33 C34 129.4(6) . . ? 
C39 C34 C35 118.2(5) . . ? 
C39 C34 C33 120.1(5) . . ? 
C35 C34 C33 121.7(5) . . ? 
C36 C35 C34 119.6(6) . . ? 
C37 C36 C35 121.7(6) . . ? 
C36 C37 C38 118.6(6) . . ? 
C37 C38 C39 121.6(6) . . ? 
C38 C39 C34 120.3(6) . . ? 
N31 B1 N11 108.9(5) . . ? 
N31 B1 N21 108.2(5) . . ? 
N11 B1 N21 109.9(5) . . ? 
C41 N41 N42 105.2(4) . . ? 
C41 N41 Cu1 130.9(4) . . ? 
N42 N41 Cu1 121.5(3) . . ? 
C43 N42 N41 111.3(4) . . ? 
N41 C41 C42 111.9(5) . . ? 
C43 C42 C41 104.7(5) . . ? 
N42 C43 C42 106.9(5) . . ? 
N42 C43 C44 121.7(5) . . ? 
C42 C43 C44 131.4(5) . . ? 
C49 C44 C45 118.9(5) . . ? 
C49 C44 C43 119.9(5) . . ? 
C45 C44 C43 121.2(5) . . ? 
C46 C45 C44 121.1(6) . . ? 
C45 C46 C47 119.2(6) . . ? 
C48 C47 C46 119.7(6) . . ? 
C47 C48 C49 120.7(7) . . ? 
C44 C49 C48 120.5(6) . . ? 
C51 O51 Cu1 132.0(4) . . ? 
O52 C51 O51 125.1(6) . . ? 
O52 C51 C52 119.0(5) . . ? 
O51 C51 C52 115.8(5) . . ? 
O53 Cu2 N91 93.5(2) . . ? 
O53 Cu2 N82 165.3(2) . . ? 
N91 Cu2 N82 89.4(2) . . ? 
O53 Cu2 N72 89.9(2) . . ? 
N91 Cu2 N72 176.4(2) . . ? 
N82 Cu2 N72 86.9(2) . . ? 
O53 Cu2 N62 103.5(2) . . ? 
N91 Cu2 N62 91.5(2) . . ? 
N82 Cu2 N62 90.8(2) . . ? 
N72 Cu2 N62 88.6(2) . . ? 
C61 N61 N62 110.5(4) . . ? 
C61 N61 B2 128.4(5) . . ? 
N62 N61 B2 121.1(4) . . ? 
C63 N62 N61 105.6(4) . . ? 
C63 N62 Cu2 143.9(3) . . ? 
N61 N62 Cu2 110.2(3) . . ? 
N61 C61 C62 108.6(5) . . ? 
C61 C62 C63 105.4(5) . . ? 
N62 C63 C62 110.0(5) . . ? 
N62 C63 C64 123.3(5) . . ? 
C62 C63 C64 126.7(5) . . ? 
C69 C64 C65 117.9(6) . . ? 
C69 C64 C63 119.9(5) . . ? 
C65 C64 C63 122.2(5) . . ? 
C66 C65 C64 120.3(6) . . ? 
C67 C66 C65 121.2(6) . . ? 
C66 C67 C68 120.1(6) . . ? 
C67 C68 C69 119.5(6) . . ? 
C64 C69 C68 121.0(6) . . ? 
C71 N71 N72 110.3(4) . . ? 
C71 N71 B2 128.2(5) . . ? 
N72 N71 B2 121.5(4) . . ? 
C73 N72 N71 105.4(4) . . ? 
C73 N72 Cu2 139.2(3) . . ? 
N71 N72 Cu2 115.0(3) . . ? 
N71 C71 C72 109.4(5) . . ? 
C71 C72 C73 105.0(5) . . ? 
N72 C73 C72 109.9(5) . . ? 
N72 C73 C74 125.8(5) . . ? 
C72 C73 C74 124.3(5) . . ? 
C75 C74 C79 117.7(5) . . ? 
C75 C74 C73 122.8(5) . . ? 
C79 C74 C73 119.4(5) . . ? 
C76 C75 C74 120.0(6) . . ? 
C75 C76 C77 121.3(6) . . ? 
C78 C77 C76 118.9(6) . . ? 
C79 C78 C77 120.1(6) . . ? 
C78 C79 C74 121.9(5) . . ? 
C81 N81 N82 109.8(4) . . ? 
C81 N81 B2 129.9(5) . . ? 
N82 N81 B2 120.3(4) . . ? 
C83 N82 N81 106.2(4) . . ? 
C83 N82 Cu2 136.7(3) . . ? 
N81 N82 Cu2 116.9(3) . . ? 
N81 C81 C82 108.4(5) . . ? 
C81 C82 C83 106.1(5) . . ? 
N82 C83 C82 109.5(5) . . ? 
N82 C83 C84 122.9(5) . . ? 
C82 C83 C84 127.5(5) . . ? 
C89 C84 C85 118.6(5) . . ? 
C89 C84 C83 122.4(5) . . ? 
C85 C84 C83 119.0(5) . . ? 
C86 C85 C84 120.7(6) . . ? 
C87 C86 C85 119.9(7) . . ? 
C88 C87 C86 120.3(6) . . ? 
C87 C88 C89 120.1(7) . . ? 
C84 C89 C88 120.5(6) . . ? 
N61 B2 N81 111.6(5) . . ? 
N61 B2 N71 110.1(5) . . ? 
N81 B2 N71 107.9(4) . . ? 
C91 N91 N92 104.7(4) . . ? 
C91 N91 Cu2 131.0(4) . . ? 
N92 N91 Cu2 124.1(3) . . ? 
C93 N92 N91 112.1(4) . . ? 
N91 C91 C92 110.8(5) . . ? 
C93 C92 C91 105.9(5) . . ? 
N92 C93 C92 106.4(5) . . ? 
N92 C93 C94 121.6(5) . . ? 
C92 C93 C94 132.0(5) . . ? 
C95 C94 C99 118.3(5) . . ? 
C95 C94 C93 120.1(5) . . ? 
C99 C94 C93 121.5(5) . . ? 
C94 C95 C96 120.7(6) . . ? 
C97 C96 C95 120.6(6) . . ? 
C96 C97 C98 118.8(6) . . ? 
C99 C98 C97 121.3(6) . . ? 
C98 C99 C94 120.3(6) . . ? 
C53 O53 Cu2 131.0(4) . . ? 
O54 C53 O53 125.1(6) . . ? 
O54 C53 C54 119.8(5) . . ? 
O53 C53 C54 115.2(6) . . ? 
  
_refine_diff_density_max    0.518 
_refine_diff_density_min   -0.566 
_refine_diff_density_rms    0.083 


#=END


data_sn331/lc65 
  
_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
Bis-[5-cyclohexylpyrazole][hydrido-tris-{3-cyclohexylpyrazol-1-yl}borato] 
copper(II) tetrafluoroborate chloroform solvate
; 
_chemical_name_common             ? 
_chemical_formula_moiety          '[C45 H68 B Cu N10][B F4][C H Cl3]' 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C46 H69 B2 Cl3 Cu F4 N10' 
_chemical_formula_weight          1029.62 
_chemical_melting_point           ? 
_chemical_compound_source         ? 
  
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0033   0.0016 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'B'  'B'   0.0013   0.0007 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'N'  'N'   0.0061   0.0033 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'F'  'F'   0.0171   0.0103 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Cu'  'Cu'   0.3201   1.2651 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Cl'  'Cl'   0.1484   0.1585 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
  
_symmetry_cell_setting            Monoclinic 
_symmetry_space_group_name_H-M    P2(1)/m 
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y+1/2, -z' 
 '-x, -y, -z' 
 'x, -y-1/2, z' 
  
_cell_length_a                    11.514(2) 
_cell_length_b                    18.291(3) 
_cell_length_c                    12.439(2) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  93.666(10) 
_cell_angle_gamma                 90.00 
_cell_volume                      2614.3(8) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     223(2) 
_cell_measurement_reflns_used     50 
_cell_measurement_theta_min       2.72 
_cell_measurement_theta_max       10.94 
  
_exptl_crystal_description        block 
_exptl_crystal_colour             blue 
_exptl_crystal_size_max           0.38 
_exptl_crystal_size_mid           0.35 
_exptl_crystal_size_min           0.33 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.308 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              1082 
_exptl_absorpt_coefficient_mu     0.627 
_exptl_absorpt_correction_type    empirical
_exptl_absorpt_correction_T_min   0.21284
_exptl_absorpt_correction_T_max   0.95510
  
_exptl_special_details 
; 
 ? 
; 
  
_diffrn_ambient_temperature       223(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device        'Siemens P4'
_diffrn_measurement_method        'theta/2 theta' 
_diffrn_standards_number          3 
_diffrn_standards_interval_count  97 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         1 
_diffrn_reflns_number             3749 
_diffrn_reflns_av_R_equivalents   0.0572 
_diffrn_reflns_av_sigmaI/netI     0.1174 
_diffrn_reflns_limit_h_min        -13 
_diffrn_reflns_limit_h_max        1 
_diffrn_reflns_limit_k_min        -1 
_diffrn_reflns_limit_k_max        21 
_diffrn_reflns_limit_l_min        -14 
_diffrn_reflns_limit_l_max        14 
_diffrn_reflns_theta_min          1.77 
_diffrn_reflns_theta_max          21.00 
_reflns_number_total              2930 
_reflns_number_observed           1418 
_reflns_observed_criterion        >2sigma(I) 
  
_computing_data_collection        'Siemens XSCANS' 
_computing_cell_refinement        'Siemens XSCANS' 
_computing_data_reduction         'Siemens SHELXTL' 
_computing_structure_solution     'SHELXS-86 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)' 
_computing_molecular_graphics     'Siemens SHELXTL' 
_computing_publication_material   'Siemens SHELXTL' 
  
_refine_special_details 
; 
 Refinement on F^2^ for ALL reflections except for 348 with very negative F^2^ 
 or flagged by the user for potential systematic errors.  Weighted R-factors 
 wR and all goodnesses of fit S are based on F^2^, conventional R-factors R 
 are based on F, with F set to zero for negative F^2^. The observed criterion 
 of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F^2^ are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 There is disorder of the BF4- anion corresponding to a slight rotation 
 about the 
 B(2)-F(1) bond; one fluorine atom was resolved into two equally occupied 
 components, 
 F(3a) and F(3b). Although  high anisotropic displacements parameters 
 indicated F(2) 
 is also affected, its location on the mirror plane made resolution 
 impossible. All C-C
 bond lengths within the cyclohexyl substituents were constrained to 
 be equal to an esd 
 of 0.03A.
; 
  
_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme 
 'calc w=1/[\s^2^(Fo^2^)+(0.1020P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     ? 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          2582 
_refine_ls_number_parameters      319 
_refine_ls_number_restraints      33 
_refine_ls_R_factor_all           0.1456 
_refine_ls_R_factor_obs           0.0721 
_refine_ls_wR_factor_all          0.2541 
_refine_ls_wR_factor_obs          0.1676 
_refine_ls_goodness_of_fit_all    1.016 
_refine_ls_goodness_of_fit_obs    1.110 
_refine_ls_restrained_S_all       1.109 
_refine_ls_restrained_S_obs       1.097 
_refine_ls_shift/esd_max          0.368 
_refine_ls_shift/esd_mean         0.025 
  
loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_thermal_displace_type 
 _atom_site_occupancy 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_group 
Cu Cu 0.14181(15) 0.2500 0.02789(14) 0.0495(6) Uani 1 d S . 
N1 N 0.0348(9) 0.2500 -0.1309(9) 0.047(3) Uani 1 d S . 
N11 N 0.0984(9) 0.2500 -0.2184(8) 0.043(3) Uani 1 d S . 
N2 N 0.2511(6) 0.3242(4) -0.0286(6) 0.043(2) Uani 1 d . . 
N21 N 0.2745(6) 0.3186(4) -0.1341(6) 0.048(2) Uani 1 d . . 
N3 N 0.0484(6) 0.3318(4) 0.0897(6) 0.044(2) Uani 1 d . . 
N31 N 0.0257(6) 0.3508(4) 0.1914(6) 0.048(2) Uani 1 d . . 
H31A H 0.0487(6) 0.3252(4) 0.2478(6) 0.058 Uiso 1 calc R . 
C11 C 0.0294(16) 0.2500 -0.3097(12) 0.074(5) Uani 1 d S . 
H11 H 0.0540(16) 0.2500 -0.3803(12) 0.089 Uiso 1 calc SR . 
C12 C -0.0849(13) 0.2500 -0.2804(12) 0.065(5) Uani 1 d S . 
H12 H -0.1532(13) 0.2500 -0.3261(12) 0.078 Uiso 1 calc SR . 
C13 C -0.0757(13) 0.2500 -0.1683(12) 0.057(4) Uani 1 d SD . 
C14 C -0.1752(11) 0.2500 -0.0962(11) 0.048(4) Uani 1 d SD . 
H14 H -0.1422(11) 0.2500 -0.0207(11) 0.058 Uiso 1 calc SR . 
C15 C -0.2522(8) 0.1824(6) -0.1119(9) 0.068(3) Uani 1 d D . 
H15A H -0.2878(8) 0.1819(6) -0.1856(9) 0.082 Uiso 1 calc R . 
H15B H -0.2044(8) 0.1383(6) -0.1019(9) 0.082 Uiso 1 calc R . 
C16 C -0.3476(8) 0.1816(6) -0.0324(10) 0.082(4) Uani 1 d D . 
H16A H -0.3122(8) 0.1795(6) 0.0413(10) 0.098 Uiso 1 calc R . 
H16B H -0.3960(8) 0.1380(6) -0.0445(10) 0.098 Uiso 1 calc R . 
C17 C -0.4235(13) 0.2500 -0.0456(17) 0.088(6) Uani 1 d SD . 
H17A H -0.4646(13) 0.2500 -0.1171(17) 0.106 Uiso 1 calc SR . 
H17B H -0.4817(13) 0.2500 0.0085(17) 0.106 Uiso 1 calc SR . 
C21 C 0.3453(8) 0.3727(6) -0.1610(8) 0.054(3) Uani 1 d . . 
H21 H 0.3747(8) 0.3801(6) -0.2289(8) 0.065 Uiso 1 calc R . 
C22 C 0.3669(8) 0.4153(6) -0.0711(8) 0.055(3) Uani 1 d . . 
H22 H 0.4117(8) 0.4583(6) -0.0670(8) 0.066 Uiso 1 calc R . 
C23 C 0.3108(8) 0.3836(5) 0.0125(7) 0.045(2) Uani 1 d D . 
C24 C 0.3151(8) 0.4024(5) 0.1285(7) 0.052(3) Uani 1 d D . 
H24 H 0.2612(8) 0.3694(5) 0.1639(7) 0.063 Uiso 1 calc R . 
C25 C 0.2771(10) 0.4804(6) 0.1477(8) 0.068(3) Uani 1 d D . 
H25A H 0.1963(10) 0.4865(6) 0.1193(8) 0.082 Uiso 1 calc R . 
H25B H 0.3256(10) 0.5137(6) 0.1083(8) 0.082 Uiso 1 calc R . 
C26 C 0.2864(10) 0.5008(6) 0.2678(8) 0.075(3) Uani 1 d D . 
H26A H 0.2643(10) 0.5521(6) 0.2763(8) 0.091 Uiso 1 calc R . 
H26B H 0.2329(10) 0.4705(6) 0.3068(8) 0.091 Uiso 1 calc R . 
C27 C 0.4109(10) 0.4891(6) 0.3147(9) 0.080(4) Uani 1 d D . 
H27A H 0.4637(10) 0.5219(6) 0.2789(9) 0.096 Uiso 1 calc R . 
H27B H 0.4157(10) 0.5009(6) 0.3917(9) 0.096 Uiso 1 calc R . 
C28 C 0.4477(10) 0.4106(7) 0.2991(8) 0.078(4) Uani 1 d D . 
H28A H 0.5284(10) 0.4042(7) 0.3276(8) 0.094 Uiso 1 calc R . 
H28B H 0.3984(10) 0.3782(7) 0.3392(8) 0.094 Uiso 1 calc R . 
C29 C 0.4376(8) 0.3901(6) 0.1804(8) 0.070(3) Uani 1 d D . 
H29A H 0.4584(8) 0.3385(6) 0.1729(8) 0.083 Uiso 1 calc R . 
H29B H 0.4931(8) 0.4192(6) 0.1420(8) 0.083 Uiso 1 calc R . 
C31 C -0.0032(8) 0.3832(5) 0.0295(8) 0.052(3) Uani 1 d . . 
H31 H -0.0036(8) 0.3853(5) -0.0460(8) 0.062 Uiso 1 calc R . 
C32 C -0.0570(8) 0.4338(6) 0.0931(9) 0.057(3) Uani 1 d . . 
H32 H -0.1001(8) 0.4748(6) 0.0685(9) 0.069 Uiso 1 calc R . 
C33 C -0.0360(8) 0.4132(6) 0.1968(8) 0.049(3) Uani 1 d D . 
C34 C -0.0716(8) 0.4452(5) 0.2986(8) 0.053(3) Uani 1 d D . 
H34 H -0.0061(8) 0.4385(5) 0.3533(8) 0.063 Uiso 1 calc R . 
C35 C -0.1755(9) 0.4073(6) 0.3395(8) 0.077(4) Uani 1 d D . 
H35A H -0.1561(9) 0.3558(6) 0.3535(8) 0.093 Uiso 1 calc R . 
H35B H -0.2396(9) 0.4088(6) 0.2838(8) 0.093 Uiso 1 calc R . 
C36 C -0.2157(11) 0.4422(6) 0.4431(9) 0.083(4) Uani 1 d D . 
H36A H -0.2868(11) 0.4178(6) 0.4635(9) 0.099 Uiso 1 calc R . 
H36B H -0.1556(11) 0.4350(6) 0.5016(9) 0.099 Uiso 1 calc R . 
C37 C -0.2390(10) 0.5231(6) 0.4285(9) 0.073(4) Uani 1 d D . 
H37A H -0.3051(10) 0.5303(6) 0.3759(9) 0.088 Uiso 1 calc R . 
H37B H -0.2590(10) 0.5444(6) 0.4971(9) 0.088 Uiso 1 calc R . 
C38 C -0.1334(10) 0.5608(6) 0.3900(8) 0.073(3) Uani 1 d D . 
H38A H -0.0703(10) 0.5580(6) 0.4465(8) 0.087 Uiso 1 calc R . 
H38B H -0.1516(10) 0.6125(6) 0.3774(8) 0.087 Uiso 1 calc R . 
C39 C -0.0913(10) 0.5272(5) 0.2853(8) 0.065(3) Uani 1 d D . 
H39A H -0.1496(10) 0.5360(5) 0.2258(8) 0.078 Uiso 1 calc R . 
H39B H -0.0186(10) 0.5507(5) 0.2675(8) 0.078 Uiso 1 calc R . 
B1 B 0.2330(15) 0.2500 -0.2007(15) 0.059(5) Uani 1 d S . 
H1 H 0.2685(15) 0.2500 -0.2711(15) 0.071 Uiso 1 calc SR . 
Cl2 Cl 0.6310(6) 0.2500 0.4250(5) 0.127(2) Uani 1 d S . 
Cl1 Cl 0.5350(4) 0.3284(2) 0.5957(3) 0.1166(14) Uani 1 d . . 
C1 C 0.5256(15) 0.2500 0.5176(12) 0.076(5) Uani 1 d S . 
H1A H 0.4487(15) 0.2500 0.4772(12) 0.091 Uiso 1 calc SR . 
B2 B 0.1855(18) 0.2500 0.3868(16) 0.065(5) Uani 1 d S . 
F1 F 0.2122(9) 0.2500 0.2862(8) 0.093(3) Uani 1 d S . 
F2 F 0.2632(11) 0.2500 0.4652(10) 0.194(8) Uani 1 d S . 
F3A F 0.1476(15) 0.3217(9) 0.4087(12) 0.112(5) Uiso 0.50 d P . 
F3B F 0.0812(14) 0.2896(8) 0.4006(11) 0.106(5) Uiso 0.50 d P . 
  
loop_ 
 _atom_site_aniso_label 
 _atom_site_aniso_U_11 
 _atom_site_aniso_U_22 
 _atom_site_aniso_U_33 
 _atom_site_aniso_U_23 
 _atom_site_aniso_U_13 
 _atom_site_aniso_U_12 
Cu 0.0466(11) 0.0503(11) 0.0520(11) 0.000 0.0051(9) 0.000 
N1 0.030(7) 0.060(7) 0.051(7) 0.000 -0.005(6) 0.000 
N11 0.043(7) 0.051(7) 0.036(7) 0.000 0.014(6) 0.000 
N2 0.036(4) 0.050(5) 0.041(5) -0.001(4) -0.002(4) 0.004(4) 
N21 0.045(5) 0.058(5) 0.043(5) 0.005(4) 0.006(4) -0.002(4) 
N3 0.045(5) 0.045(5) 0.042(5) 0.009(4) 0.007(4) 0.007(4) 
N31 0.047(5) 0.062(6) 0.036(5) 0.012(4) 0.001(4) 0.009(5) 
C11 0.102(15) 0.079(12) 0.037(9) 0.000 -0.039(10) 0.000 
C12 0.030(9) 0.107(13) 0.055(11) 0.000 -0.014(8) 0.000 
C13 0.067(12) 0.047(9) 0.057(11) 0.000 -0.002(9) 0.000 
C14 0.044(8) 0.055(9) 0.044(8) 0.000 -0.006(7) 0.000 
C15 0.049(7) 0.060(6) 0.094(8) -0.010(6) -0.015(6) -0.013(6) 
C16 0.043(7) 0.062(7) 0.141(11) -0.001(8) 0.011(7) -0.013(6) 
C17 0.048(10) 0.056(10) 0.159(18) 0.000 0.001(11) 0.000 
C21 0.051(6) 0.065(7) 0.048(7) 0.020(6) 0.008(5) -0.001(6) 
C22 0.051(7) 0.057(7) 0.056(7) 0.003(6) -0.009(6) -0.011(5) 
C23 0.034(5) 0.058(7) 0.043(6) 0.006(5) 0.004(5) 0.007(5) 
C24 0.053(6) 0.053(6) 0.050(6) 0.011(5) -0.004(5) 0.000(5) 
C25 0.067(8) 0.071(8) 0.064(8) 0.007(6) -0.012(6) 0.008(6) 
C26 0.092(10) 0.068(8) 0.065(8) -0.005(6) -0.007(7) 0.004(7) 
C27 0.087(10) 0.088(9) 0.065(8) -0.022(7) 0.004(7) -0.033(8) 
C28 0.078(9) 0.102(10) 0.052(7) -0.011(7) -0.021(6) -0.015(8) 
C29 0.057(7) 0.070(8) 0.079(8) 0.015(6) -0.015(6) -0.001(6) 
C31 0.050(6) 0.061(7) 0.044(6) 0.007(6) -0.007(5) 0.003(5) 
C32 0.046(6) 0.059(7) 0.066(8) -0.007(6) 0.002(6) 0.012(6) 
C33 0.045(6) 0.060(7) 0.043(7) -0.007(6) 0.002(5) 0.008(5) 
C34 0.038(6) 0.060(7) 0.060(7) 0.006(6) -0.002(5) 0.017(5) 
C35 0.078(8) 0.075(8) 0.083(8) -0.002(7) 0.038(7) -0.008(7) 
C36 0.094(10) 0.085(9) 0.071(8) -0.006(7) 0.026(7) 0.004(8) 
C37 0.075(8) 0.089(9) 0.058(7) -0.012(7) 0.018(6) 0.036(7) 
C38 0.096(9) 0.053(7) 0.070(8) -0.010(6) 0.018(7) 0.005(7) 
C39 0.076(8) 0.066(8) 0.053(7) -0.003(6) 0.013(6) 0.009(6) 
B1 0.054(12) 0.060(11) 0.064(12) 0.000 0.017(10) 0.000 
Cl2 0.179(6) 0.083(3) 0.127(5) 0.000 0.074(4) 0.000 
Cl1 0.137(3) 0.104(3) 0.111(3) -0.040(2) 0.031(2) -0.021(3) 
C1 0.098(13) 0.062(10) 0.066(11) 0.000 -0.019(10) 0.000 
B2 0.078(14) 0.055(12) 0.059(13) 0.000 -0.020(12) 0.000 
F1 0.102(8) 0.109(8) 0.069(7) 0.000 0.002(6) 0.000 
F2 0.104(10) 0.380(25) 0.090(9) 0.000 -0.054(8) 0.000 
  
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
  
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
Cu N2 2.008(7) . ? 
Cu N3 2.022(7) . ? 
Cu N1 2.260(11) . ? 
N1 C13 1.33(2) . ? 
N1 N11 1.350(13) . ? 
N11 C11 1.34(2) . ? 
N11 B1 1.55(2) . ? 
N2 N21 1.360(9) . ? 
N2 C23 1.367(11) . ? 
N21 C21 1.338(11) . ? 
N21 B1 1.562(13) . ? 
N3 C31 1.320(11) . ? 
N3 N31 1.354(9) . ? 
N31 C33 1.349(11) . ? 
C11 C12 1.39(2) . ? 
C12 C13 1.39(2) . ? 
C13 C14 1.50(2) . ? 
C14 C15 1.527(11) . ? 
C15 C16 1.524(12) . ? 
C16 C17 1.528(12) . ? 
C21 C22 1.372(12) . ? 
C22 C23 1.387(12) . ? 
C23 C24 1.480(11) . ? 
C24 C25 1.515(12) . ? 
C24 C29 1.531(11) . ? 
C25 C26 1.537(12) . ? 
C26 C27 1.528(12) . ? 
C27 C28 1.514(13) . ? 
C28 C29 1.520(12) . ? 
C31 C32 1.389(12) . ? 
C32 C33 1.351(12) . ? 
C33 C34 1.476(12) . ? 
C34 C35 1.500(11) . ? 
C34 C39 1.523(12) . ? 
C35 C36 1.535(12) . ? 
C36 C37 1.513(13) . ? 
C37 C38 1.502(12) . ? 
C38 C39 1.545(11) . ? 
Cl2 C1 1.73(2) . ? 
Cl1 C1 1.732(9) . ? 
B2 F2 1.28(2) . ? 
B2 F1 1.31(2) . ? 
B2 F3A 1.41(2) . ? 
B2 F3B 1.42(2) . ? 
  
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
N2 Cu N2 85.0(4) . 4_565 ? 
N2 Cu N3 89.6(3) . . ? 
N2 Cu N3 173.3(3) . 4_565 ? 
N3 Cu N3 95.4(4) . 4_565 ? 
N2 Cu N1 90.8(3) . . ? 
N3 Cu N1 93.4(3) . . ? 
C13 N1 N11 106.0(11) . . ? 
C13 N1 Cu 139.8(9) . . ? 
N11 N1 Cu 114.3(8) . . ? 
C11 N11 N1 111.0(12) . . ? 
C11 N11 B1 130.7(13) . . ? 
N1 N11 B1 118.3(11) . . ? 
N21 N2 C23 107.2(7) . . ? 
N21 N2 Cu 117.0(6) . . ? 
C23 N2 Cu 135.9(6) . . ? 
C21 N21 N2 110.3(8) . . ? 
C21 N21 B1 129.2(9) . . ? 
N2 N21 B1 120.0(9) . . ? 
C31 N3 N31 103.9(7) . . ? 
C31 N3 Cu 122.9(6) . . ? 
N31 N3 Cu 133.2(6) . . ? 
C33 N31 N3 113.5(7) . . ? 
N11 C11 C12 107.4(14) . . ? 
C11 C12 C13 104.5(13) . . ? 
N1 C13 C12 111.2(12) . . ? 
N1 C13 C14 122.9(13) . . ? 
C12 C13 C14 125.9(14) . . ? 
C13 C14 C15 112.5(7) . . ? 
C15 C14 C15 108.1(11) 4_565 . ? 
C16 C15 C14 111.2(9) . . ? 
C15 C16 C17 110.7(11) . . ? 
C16 C17 C16 109.8(12) 4_565 . ? 
N21 C21 C22 107.3(8) . . ? 
C21 C22 C23 107.7(9) . . ? 
N2 C23 C22 107.4(8) . . ? 
N2 C23 C24 122.2(8) . . ? 
C22 C23 C24 130.2(9) . . ? 
C23 C24 C25 112.4(8) . . ? 
C23 C24 C29 110.5(8) . . ? 
C25 C24 C29 109.9(9) . . ? 
C24 C25 C26 112.3(8) . . ? 
C27 C26 C25 110.0(9) . . ? 
C28 C27 C26 110.3(10) . . ? 
C29 C28 C27 110.7(10) . . ? 
C28 C29 C24 112.6(9) . . ? 
N3 C31 C32 110.7(8) . . ? 
C33 C32 C31 107.4(9) . . ? 
N31 C33 C32 104.5(8) . . ? 
N31 C33 C34 123.7(9) . . ? 
C32 C33 C34 131.8(10) . . ? 
C33 C34 C35 112.2(8) . . ? 
C33 C34 C39 110.2(8) . . ? 
C35 C34 C39 112.1(8) . . ? 
C34 C35 C36 112.4(9) . . ? 
C37 C36 C35 111.5(9) . . ? 
C38 C37 C36 110.3(9) . . ? 
C37 C38 C39 112.9(9) . . ? 
C34 C39 C38 110.6(8) . . ? 
N11 B1 N21 110.2(8) . . ? 
N21 B1 N21 106.9(12) . 4_565 ? 
Cl1 C1 Cl1 111.8(9) . 4_565 ? 
Cl1 C1 Cl2 110.7(7) . . ? 
F2 B2 F1 122.2(19) . . ? 
F2 B2 F3A 93.6(11) . . ? 
F1 B2 F3A 106.2(11) . . ? 
F2 B2 F3B 117.5(15) . . ? 
F1 B2 F3B 111.6(14) . . ? 
F3A B2 F3B 100.1(17) 4_565 . ? 
  
_refine_diff_density_max    0.564 
_refine_diff_density_min   -0.520 
_refine_diff_density_rms    0.076 


#=END



data_sy345/lc80 
  
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
[5-Cyclohexylpyrazole][5-cyclohexylpyrazolato][hydrido-tris-{3-cyclohexyl-
pyrazol-1-yl}borato]copper(II)
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C45 H66 B Cu N10' 
_chemical_formula_weight          821.43 
  
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0033   0.0016 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'B'  'B'   0.0013   0.0007 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'N'  'N'   0.0061   0.0033 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Cu'  'Cu'   0.3201   1.2651 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
  
_symmetry_cell_setting            Monoclinic 
_symmetry_space_group_name_H-M    P2(1)/n 
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x+1/2, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x-1/2, -y-1/2, z-1/2' 
  
_cell_length_a                    11.4095(17) 
_cell_length_b                    21.315(4) 
_cell_length_c                    18.692(4) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  95.435(15) 
_cell_angle_gamma                 90.00 
_cell_volume                      4525.5(14) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     223(2) 
_cell_measurement_reflns_used     39 
_cell_measurement_theta_min       2.24 
_cell_measurement_theta_max       11.00 
  
_exptl_crystal_description        block 
_exptl_crystal_colour             blue 
_exptl_crystal_size_max           0.38 
_exptl_crystal_size_mid           0.40 
_exptl_crystal_size_min           0.38 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.206 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1760 
_exptl_absorpt_coefficient_mu     0.525 
_exptl_absorpt_correction_type    empirical 
_exptl_absorpt_correction_T_min   0.24587 
_exptl_absorpt_correction_T_max   0.96203 
_exptl_absorpt_process_details    ? 
  
_exptl_special_details 
; 
 ? 
; 
  
_diffrn_ambient_temperature       223(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Bruker P4' 
_diffrn_measurement_method        theta/2theta 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          3 
_diffrn_standards_interval_count  97 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         2 
_diffrn_reflns_number             7882 
_diffrn_reflns_av_R_equivalents   0.0543 
_diffrn_reflns_av_sigmaI/netI     0.1614 
_diffrn_reflns_limit_h_min        -1 
_diffrn_reflns_limit_h_max        12 
_diffrn_reflns_limit_k_min        -1 
_diffrn_reflns_limit_k_max        23 
_diffrn_reflns_limit_l_min        -20 
_diffrn_reflns_limit_l_max        20 
_diffrn_reflns_theta_min          1.91 
_diffrn_reflns_theta_max          23.00 
_reflns_number_total              6306 
_reflns_number_gt                 2084 
_reflns_threshold_expression      >2sigma(I) 
  
_computing_data_collection        'Bruker XSCANS' 
_computing_cell_refinement        'Bruker XSCANS' 
_computing_data_reduction         'Bruker SHELXTL' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'Bruker SHELXTL' 
_computing_publication_material   'Bruker SHELXTL' 
  
_refine_special_details 
; 
 Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F^2^, conventional R-factors R are based 
 on F, with F set to zero for negative F^2^. The threshold expression of 
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F^2^ are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 

 All C-C bond lengths within the cyclohexyl substituents were constrained to 
 be equal to an esd of 0.03A.
; 
  
_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
 'calc w=1/[\s^2^(Fo^2^)+(0.1108P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          6306 
_refine_ls_number_parameters      514 
_refine_ls_number_restraints      168 
_refine_ls_R_factor_all           0.1988 
_refine_ls_R_factor_gt            0.0734 
_refine_ls_wR_factor_ref          0.2647 
_refine_ls_wR_factor_gt           0.1719 
_refine_ls_goodness_of_fit_ref    0.922 
_refine_ls_restrained_S_all       0.918 
_refine_ls_shift/su_max           0.011 
_refine_ls_shift/su_mean          0.001 
  
loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_adp_type 
 _atom_site_occupancy 
 _atom_site_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Cu Cu -0.55141(10) 0.33570(6) -0.34055(6) 0.0610(4) Uani 1 1 d . . . 
N1 N -0.5259(7) 0.3654(3) -0.2401(4) 0.056(2) Uani 1 1 d D . . 
N11 N -0.4206(6) 0.3601(3) -0.1975(4) 0.056(2) Uani 1 1 d D . . 
N2 N -0.3909(6) 0.3641(3) -0.3619(4) 0.059(2) Uani 1 1 d D . . 
N21 N -0.2984(7) 0.3656(4) -0.3086(4) 0.065(2) Uani 1 1 d D . . 
N3 N -0.7015(6) 0.2907(4) -0.3195(4) 0.063(2) Uani 1 1 d D . . 
N31 N -0.7980(7) 0.3005(4) -0.3684(4) 0.066(2) Uani 1 1 d D . . 
N4 N -0.5805(7) 0.2918(4) -0.4385(4) 0.061(2) Uani 1 1 d D . . 
N41 N -0.6887(6) 0.3035(3) -0.4755(4) 0.058(2) Uani 1 1 d D . . 
N5 N -0.6507(7) 0.4173(4) -0.3846(4) 0.074(2) Uani 1 1 d D . . 
N51 N -0.7561(7) 0.4038(4) -0.4234(4) 0.073(3) Uani 1 1 d D . . 
C11 C -0.6058(9) 0.3892(5) -0.1998(6) 0.072(3) Uani 1 1 d D . . 
H11 H -0.6850 0.3970 -0.2160 0.087 Uiso 1 1 calc R . . 
C12 C -0.5558(9) 0.4007(5) -0.1319(5) 0.072(3) Uani 1 1 d D . . 
H12 H -0.5927 0.4174 -0.0932 0.087 Uiso 1 1 calc R . . 
C13 C -0.4389(8) 0.3826(4) -0.1319(4) 0.059(3) Uani 1 1 d D . . 
C14 C -0.3423(8) 0.3873(4) -0.0728(4) 0.061(3) Uani 1 1 d D . . 
H14 H -0.2769 0.3610 -0.0868 0.073 Uiso 1 1 calc R . . 
C15 C -0.3750(8) 0.3622(5) -0.0010(4) 0.077(3) Uani 1 1 d D . . 
H15A H -0.4440 0.3850 0.0127 0.093 Uiso 1 1 calc R . . 
H15B H -0.3965 0.3179 -0.0066 0.093 Uiso 1 1 calc R . . 
C16 C -0.2756(10) 0.3686(5) 0.0584(5) 0.084(4) Uani 1 1 d D . . 
H16A H -0.3040 0.3561 0.1041 0.101 Uiso 1 1 calc R . . 
H16B H -0.2114 0.3403 0.0487 0.101 Uiso 1 1 calc R . . 
C17 C -0.2294(10) 0.4343(5) 0.0648(5) 0.088(4) Uani 1 1 d D . . 
H17A H -0.2904 0.4618 0.0813 0.106 Uiso 1 1 calc R . . 
H17B H -0.1615 0.4355 0.1011 0.106 Uiso 1 1 calc R . . 
C18 C -0.1932(10) 0.4588(5) -0.0048(5) 0.097(4) Uani 1 1 d D . . 
H18A H -0.1259 0.4347 -0.0187 0.117 Uiso 1 1 calc R . . 
H18B H -0.1689 0.5028 0.0011 0.117 Uiso 1 1 calc R . . 
C19 C -0.2949(10) 0.4540(5) -0.0639(5) 0.092(4) Uani 1 1 d D . . 
H19A H -0.3586 0.4820 -0.0523 0.110 Uiso 1 1 calc R . . 
H19B H -0.2679 0.4680 -0.1095 0.110 Uiso 1 1 calc R . . 
C21 C -0.3490(10) 0.3845(5) -0.4216(5) 0.080(3) Uani 1 1 d D . . 
H21 H -0.3932 0.3876 -0.4665 0.096 Uiso 1 1 calc R . . 
C22 C -0.2331(10) 0.4005(5) -0.4088(5) 0.084(4) Uani 1 1 d D . . 
H22 H -0.1838 0.4159 -0.4424 0.100 Uiso 1 1 calc R . . 
C23 C -0.2031(8) 0.3896(5) -0.3367(5) 0.064(3) Uani 1 1 d D . . 
C24 C -0.0876(9) 0.3976(5) -0.2934(5) 0.075(3) Uani 1 1 d D . . 
H24 H -0.0262 0.3809 -0.3222 0.090 Uiso 1 1 calc R . . 
C25 C -0.0613(13) 0.4649(6) -0.2798(9) 0.211(11) Uani 1 1 d D . . 
H25A H -0.1206 0.4826 -0.2509 0.253 Uiso 1 1 calc R . . 
H25B H -0.0664 0.4873 -0.3257 0.253 Uiso 1 1 calc R . . 
C26 C 0.0629(12) 0.4750(7) -0.2399(8) 0.175(9) Uani 1 1 d D . . 
H26A H 0.1234 0.4583 -0.2686 0.210 Uiso 1 1 calc R . . 
H26B H 0.0777 0.5198 -0.2318 0.210 Uiso 1 1 calc R . . 
C27 C 0.0660(12) 0.4415(6) -0.1703(6) 0.124(5) Uani 1 1 d D . . 
H27A H 0.1430 0.4478 -0.1433 0.148 Uiso 1 1 calc R . . 
H27B H 0.0059 0.4589 -0.1419 0.148 Uiso 1 1 calc R . . 
C28 C 0.0447(10) 0.3734(7) -0.1811(7) 0.134(6) Uani 1 1 d D . . 
H28A H 0.0470 0.3522 -0.1345 0.160 Uiso 1 1 calc R . . 
H28B H 0.1063 0.3553 -0.2079 0.160 Uiso 1 1 calc R . . 
C29 C -0.0768(10) 0.3637(8) -0.2233(6) 0.155(7) Uani 1 1 d D . . 
H29A H -0.0894 0.3187 -0.2321 0.186 Uiso 1 1 calc R . . 
H29B H -0.1382 0.3785 -0.1941 0.186 Uiso 1 1 calc R . . 
C31 C -0.8840(9) 0.2653(5) -0.3465(6) 0.077(3) Uani 1 1 d D . . 
H31 H -0.9602 0.2625 -0.3702 0.093 Uiso 1 1 calc R . . 
C32 C -0.8471(9) 0.2342(5) -0.2856(6) 0.078(3) Uani 1 1 d D . . 
H32 H -0.8923 0.2077 -0.2589 0.094 Uiso 1 1 calc R . . 
C33 C -0.7288(8) 0.2493(5) -0.2703(5) 0.062(3) Uani 1 1 d D . . 
C34 C -0.6386(8) 0.2264(4) -0.2157(4) 0.061(3) Uani 1 1 d D . . 
H34 H -0.5914 0.2630 -0.1975 0.074 Uiso 1 1 calc R . . 
C35 C -0.5563(10) 0.1820(6) -0.2502(5) 0.104(4) Uani 1 1 d D . . 
H35A H -0.5230 0.2037 -0.2898 0.124 Uiso 1 1 calc R . . 
H35B H -0.6017 0.1460 -0.2704 0.124 Uiso 1 1 calc R . . 
C36 C -0.4563(10) 0.1581(7) -0.1975(6) 0.111(5) Uani 1 1 d D . . 
H36A H -0.4092 0.1277 -0.2217 0.133 Uiso 1 1 calc R . . 
H36B H -0.4049 0.1933 -0.1815 0.133 Uiso 1 1 calc R . . 
C37 C -0.5025(11) 0.1278(5) -0.1334(6) 0.094(4) Uani 1 1 d D . . 
H37A H -0.5445 0.0892 -0.1484 0.113 Uiso 1 1 calc R . . 
H37B H -0.4365 0.1166 -0.0984 0.113 Uiso 1 1 calc R . . 
C38 C -0.5836(10) 0.1709(6) -0.0993(5) 0.092(4) Uani 1 1 d D . . 
H38A H -0.5387 0.2069 -0.0791 0.110 Uiso 1 1 calc R . . 
H38B H -0.6161 0.1489 -0.0596 0.110 Uiso 1 1 calc R . . 
C39 C -0.6845(9) 0.1943(6) -0.1516(5) 0.089(4) Uani 1 1 d D . . 
H39A H -0.7347 0.1589 -0.1681 0.107 Uiso 1 1 calc R . . 
H39B H -0.7325 0.2240 -0.1269 0.107 Uiso 1 1 calc R . . 
C41 C -0.6895(9) 0.2759(5) -0.5396(5) 0.067(3) Uani 1 1 d D . . 
H41 H -0.7523 0.2771 -0.5759 0.080 Uiso 1 1 calc R . . 
C42 C -0.5849(9) 0.2455(4) -0.5442(5) 0.064(3) Uani 1 1 d D . . 
H42 H -0.5621 0.2228 -0.5837 0.077 Uiso 1 1 calc R . . 
C43 C -0.5193(8) 0.2550(4) -0.4789(5) 0.058(3) Uani 1 1 d D . . 
C44 C -0.4064(8) 0.2269(4) -0.4496(5) 0.063(3) Uani 1 1 d D . . 
H44 H -0.3821 0.2479 -0.4033 0.076 Uiso 1 1 calc R . . 
C45 C -0.3065(8) 0.2347(5) -0.4977(5) 0.073(3) Uani 1 1 d D . . 
H45A H -0.3295 0.2159 -0.5447 0.088 Uiso 1 1 calc R . . 
H45B H -0.2919 0.2795 -0.5048 0.088 Uiso 1 1 calc R . . 
C46 C -0.1940(9) 0.2036(5) -0.4642(7) 0.100(4) Uani 1 1 d D . . 
H46A H -0.1329 0.2073 -0.4975 0.120 Uiso 1 1 calc R . . 
H46B H -0.1665 0.2258 -0.4199 0.120 Uiso 1 1 calc R . . 
C47 C -0.2107(10) 0.1354(5) -0.4472(6) 0.091(4) Uani 1 1 d D . . 
H47A H -0.1377 0.1186 -0.4226 0.109 Uiso 1 1 calc R . . 
H47B H -0.2284 0.1119 -0.4919 0.109 Uiso 1 1 calc R . . 
C48 C -0.3097(9) 0.1272(5) -0.4001(5) 0.082(3) Uani 1 1 d D . . 
H48A H -0.2878 0.1466 -0.3532 0.099 Uiso 1 1 calc R . . 
H48B H -0.3229 0.0824 -0.3924 0.099 Uiso 1 1 calc R . . 
C49 C -0.4224(8) 0.1570(4) -0.4341(5) 0.066(3) Uani 1 1 d D . . 
H49A H -0.4845 0.1519 -0.4018 0.080 Uiso 1 1 calc R . . 
H49B H -0.4475 0.1352 -0.4791 0.080 Uiso 1 1 calc R . . 
C51 C -0.8066(10) 0.4577(5) -0.4439(6) 0.091(4) Uani 1 1 d D . . 
H51 H -0.8786 0.4613 -0.4725 0.109 Uiso 1 1 calc R . . 
C52 C -0.7405(10) 0.5071(5) -0.4180(6) 0.093(4) Uani 1 1 d D . . 
H52 H -0.7574 0.5500 -0.4244 0.112 Uiso 1 1 calc R . . 
C53 C -0.6419(9) 0.4803(5) -0.3799(5) 0.082(3) Uani 1 1 d D . . 
C54 C -0.5364(9) 0.5099(4) -0.3410(5) 0.070(3) Uani 1 1 d D . . 
H54 H -0.4833 0.4760 -0.3217 0.084 Uiso 1 1 calc R . . 
C55 C -0.4700(10) 0.5491(5) -0.3921(5) 0.088(4) Uani 1 1 d D . . 
H55A H -0.5216 0.5824 -0.4132 0.105 Uiso 1 1 calc R . . 
H55B H -0.4470 0.5225 -0.4312 0.105 Uiso 1 1 calc R . . 
C56 C -0.3600(10) 0.5784(6) -0.3521(6) 0.106(4) Uani 1 1 d D . . 
H56A H -0.3062 0.5450 -0.3341 0.127 Uiso 1 1 calc R . . 
H56B H -0.3195 0.6040 -0.3857 0.127 Uiso 1 1 calc R . . 
C57 C -0.3899(12) 0.6185(6) -0.2904(7) 0.114(5) Uani 1 1 d D . . 
H57A H -0.4372 0.6545 -0.3086 0.137 Uiso 1 1 calc R . . 
H57B H -0.3174 0.6345 -0.2644 0.137 Uiso 1 1 calc R . . 
C58 C -0.4579(10) 0.5804(5) -0.2403(6) 0.104(4) Uani 1 1 d D . . 
H58A H -0.4809 0.6078 -0.2019 0.124 Uiso 1 1 calc R . . 
H58B H -0.4063 0.5477 -0.2180 0.124 Uiso 1 1 calc R . . 
C59 C -0.5693(9) 0.5493(5) -0.2778(5) 0.087(4) Uani 1 1 d D . . 
H59A H -0.6059 0.5226 -0.2435 0.104 Uiso 1 1 calc R . . 
H59B H -0.6262 0.5817 -0.2949 0.104 Uiso 1 1 calc R . . 
B1 B -0.7864(10) 0.3353(5) -0.4387(5) 0.067(3) Uani 1 1 d D . . 
H1 H -0.8614 0.3325 -0.4699 0.080 Uiso 1 1 calc R . . 
  
loop_ 
 _atom_site_aniso_label 
 _atom_site_aniso_U_11 
 _atom_site_aniso_U_22 
 _atom_site_aniso_U_33 
 _atom_site_aniso_U_23 
 _atom_site_aniso_U_13 
 _atom_site_aniso_U_12 
Cu 0.0598(8) 0.0636(8) 0.0587(7) -0.0016(6) 0.0011(6) -0.0001(7) 
N1 0.056(5) 0.062(5) 0.050(4) 0.003(4) 0.003(4) -0.012(4) 
N11 0.058(5) 0.060(5) 0.049(4) 0.001(4) 0.000(4) -0.011(4) 
N2 0.056(5) 0.062(5) 0.059(5) -0.001(4) -0.001(4) -0.007(4) 
N21 0.063(5) 0.069(5) 0.062(5) 0.001(4) -0.002(4) -0.015(5) 
N3 0.045(5) 0.073(6) 0.069(5) -0.008(5) -0.003(4) -0.002(4) 
N31 0.060(6) 0.074(6) 0.062(5) -0.006(4) -0.003(5) 0.002(5) 
N4 0.068(6) 0.058(5) 0.055(5) -0.004(4) 0.000(4) -0.001(5) 
N41 0.054(5) 0.061(5) 0.058(5) -0.001(4) -0.006(4) -0.002(4) 
N5 0.075(6) 0.068(6) 0.074(6) -0.009(5) -0.013(5) 0.008(5) 
N51 0.079(6) 0.065(6) 0.071(5) 0.001(4) -0.013(5) 0.018(5) 
C11 0.063(7) 0.068(7) 0.087(8) 0.002(6) 0.011(6) 0.005(6) 
C12 0.077(8) 0.085(8) 0.057(6) -0.003(6) 0.012(6) 0.013(7) 
C13 0.071(7) 0.053(6) 0.052(6) -0.004(5) -0.006(5) -0.002(6) 
C14 0.064(7) 0.058(6) 0.060(6) -0.004(5) 0.003(5) 0.012(5) 
C15 0.077(8) 0.098(8) 0.059(6) -0.008(6) 0.018(6) -0.026(7) 
C16 0.100(9) 0.093(9) 0.058(6) 0.003(6) -0.003(6) -0.011(7) 
C17 0.107(9) 0.082(8) 0.069(7) -0.024(6) -0.021(7) 0.017(7) 
C18 0.110(10) 0.090(9) 0.086(8) 0.005(7) -0.021(8) -0.033(8) 
C19 0.100(9) 0.075(8) 0.094(8) 0.023(6) -0.024(7) -0.022(7) 
C21 0.092(9) 0.093(9) 0.053(6) 0.019(6) 0.001(6) -0.017(7) 
C22 0.082(8) 0.109(9) 0.059(7) 0.010(6) 0.001(6) -0.037(8) 
C23 0.059(7) 0.079(7) 0.053(6) -0.002(5) 0.007(5) -0.008(6) 
C24 0.064(7) 0.091(8) 0.071(7) -0.003(6) 0.010(6) -0.007(7) 
C25 0.203(18) 0.106(12) 0.29(2) 0.071(13) -0.170(17) -0.057(12) 
C26 0.137(14) 0.145(14) 0.223(17) 0.110(13) -0.089(13) -0.075(11) 
C27 0.121(12) 0.117(12) 0.124(11) -0.048(10) -0.035(9) -0.009(10) 
C28 0.098(11) 0.167(15) 0.130(12) 0.042(11) -0.021(9) -0.058(11) 
C29 0.101(11) 0.242(18) 0.113(10) 0.074(11) -0.041(9) -0.101(12) 
C31 0.053(7) 0.089(9) 0.090(8) -0.019(7) 0.008(6) -0.002(7) 
C32 0.059(7) 0.103(9) 0.075(7) -0.008(7) 0.017(6) -0.016(7) 
C33 0.057(7) 0.068(7) 0.064(6) -0.017(6) 0.017(5) -0.007(6) 
C34 0.069(7) 0.063(7) 0.053(6) -0.001(5) 0.011(5) 0.003(6) 
C35 0.089(9) 0.155(12) 0.069(7) 0.006(8) 0.020(7) 0.037(9) 
C36 0.100(10) 0.158(13) 0.077(8) 0.030(9) 0.024(7) 0.041(10) 
C37 0.110(10) 0.089(9) 0.083(8) -0.002(7) 0.004(7) 0.027(8) 
C38 0.112(10) 0.109(10) 0.056(6) 0.024(7) 0.013(7) -0.009(9) 
C39 0.087(9) 0.110(9) 0.074(7) -0.014(7) 0.028(7) 0.003(8) 
C41 0.084(8) 0.070(7) 0.046(6) -0.001(5) -0.003(6) -0.022(7) 
C42 0.062(7) 0.068(7) 0.064(6) -0.006(5) 0.009(6) 0.003(6) 
C43 0.057(7) 0.061(7) 0.055(6) 0.002(5) 0.004(5) -0.018(6) 
C44 0.063(7) 0.059(7) 0.068(6) 0.001(5) 0.010(5) -0.006(6) 
C45 0.061(7) 0.089(8) 0.074(7) 0.008(6) 0.029(6) -0.011(6) 
C46 0.062(8) 0.112(11) 0.131(11) -0.016(9) 0.037(7) 0.000(8) 
C47 0.081(9) 0.082(9) 0.114(10) 0.024(7) 0.025(7) 0.012(7) 
C48 0.084(8) 0.096(9) 0.071(7) 0.006(6) 0.028(6) -0.001(7) 
C49 0.071(7) 0.068(7) 0.062(6) -0.001(5) 0.018(5) 0.001(6) 
C51 0.089(9) 0.076(8) 0.100(8) -0.003(7) -0.033(7) 0.014(7) 
C52 0.107(10) 0.058(7) 0.108(9) -0.011(7) -0.023(8) 0.016(7) 
C53 0.097(9) 0.078(8) 0.067(7) 0.006(6) -0.016(6) 0.005(7) 
C54 0.090(8) 0.045(6) 0.071(6) -0.004(5) -0.013(6) 0.001(6) 
C55 0.114(10) 0.075(8) 0.072(7) 0.005(6) 0.002(7) 0.004(8) 
C56 0.122(11) 0.084(9) 0.112(10) 0.000(8) 0.009(9) -0.022(9) 
C57 0.137(13) 0.077(9) 0.123(11) 0.009(9) -0.019(10) -0.035(9) 
C58 0.134(12) 0.073(8) 0.098(9) -0.027(7) -0.022(9) 0.003(8) 
C59 0.119(10) 0.066(7) 0.073(7) -0.014(6) -0.001(7) 0.004(7) 
B1 0.066(8) 0.066(8) 0.065(7) -0.005(7) -0.013(6) 0.009(7) 
  
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
  
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
Cu N1 1.976(7) . ? 
Cu N2 2.004(8) . ? 
Cu N3 2.033(8) . ? 
Cu N4 2.055(7) . ? 
Cu N5 2.194(8) . ? 
N1 C11 1.336(10) . ? 
N1 N11 1.382(8) . ? 
N11 C13 1.352(9) . ? 
N2 C21 1.328(10) . ? 
N2 N21 1.381(8) . ? 
N21 C23 1.353(10) . ? 
N3 C33 1.333(10) . ? 
N3 N31 1.379(8) . ? 
N31 C31 1.330(10) . ? 
N31 B1 1.526(10) . ? 
N4 C43 1.331(10) . ? 
N4 N41 1.380(8) . ? 
N41 C41 1.334(9) . ? 
N41 B1 1.522(10) . ? 
N5 C53 1.348(10) . ? 
N5 N51 1.376(9) . ? 
N51 C51 1.325(10) . ? 
N51 B1 1.522(10) . ? 
C11 C12 1.364(11) . ? 
C12 C13 1.388(11) . ? 
C13 C14 1.488(9) . ? 
C14 C15 1.522(9) . ? 
C14 C19 1.524(10) . ? 
C15 C16 1.517(10) . ? 
C16 C17 1.497(10) . ? 
C17 C18 1.497(10) . ? 
C18 C19 1.527(10) . ? 
C21 C22 1.365(12) . ? 
C22 C23 1.379(10) . ? 
C23 C24 1.489(10) . ? 
C24 C25 1.483(11) . ? 
C24 C29 1.491(10) . ? 
C25 C26 1.552(11) . ? 
C26 C27 1.482(11) . ? 
C27 C28 1.482(11) . ? 
C28 C29 1.542(10) . ? 
C31 C32 1..349(11) . ? 
C32 C33 1.390(11) . ? 
C33 C34 1.464(10) . ? 
C34 C39 1.515(10) . ? 
C34 C35 1.519(10) . ? 
C35 C36 1.523(10) . ? 
C36 C37 1.500(11) . ? 
C37 C38 1.489(11) . ? 
C38 C39 1.522(10) . ? 
C41 C42 1.368(11) . ? 
C42 C43 1.386(10) . ? 
C43 C44 1.478(10) . ? 
C44 C45 1.526(10) . ? 
C44 C49 1.532(10) . ? 
C45 C46 1.525(10) . ? 
C46 C47 1.503(11) . ? 
C47 C48 1.506(10) . ? 
C48 C49 1.518(10) . ? 
C51 C52 1.356(11) . ? 
C52 C53 1.396(11) . ? 
C53 C54 1.487(10) . ? 
C54 C55 1.522(10) . ? 
C54 C59 1.525(10) . ? 
C55 C56 1.531(11) . ? 
C56 C57 1.501(11) . ? 
C57 C58 1.509(11) . ? 
C58 C59 1.541(10) . ? 
  
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
N1 Cu N2 92.2(3) . . ? 
N1 Cu N3 91.0(3) . . ? 
N2 Cu N3 169.4(3) . . ? 
N1 Cu N4 171.5(3) . . ? 
N2 Cu N4 91.9(3) . . ? 
N3 Cu N4 83.7(3) . . ? 
N1 Cu N5 97.3(3) . . ? 
N2 Cu N5 97.8(3) . . ? 
N3 Cu N5 91.9(3) . . ? 
N4 Cu N5 89.6(3) . . ? 
C11 N1 N11 108.0(7) . . ? 
C11 N1 Cu 127.6(6) . . ? 
N11 N1 Cu 124.2(6) . . ? 
C13 N11 N1 107.0(7) . . ? 
C21 N2 N21 106.7(8) . . ? 
C21 N2 Cu 132.4(6) . . ? 
N21 N2 Cu 120.9(6) . . ? 
C23 N21 N2 108.4(7) . . ? 
C33 N3 N31 109.4(8) . . ? 
C33 N3 Cu 134.6(6) . . ? 
N31 N3 Cu 115.8(7) . . ? 
C31 N31 N3 106.1(8) . . ? 
C31 N31 B1 131.8(8) . . ? 
N3 N31 B1 121.0(8) . . ? 
C43 N4 N41 108.4(7) . . ? 
C43 N4 Cu 136.4(6) . . ? 
N41 N4 Cu 115.2(6) . . ? 
C41 N41 N4 107.4(8) . . ? 
C41 N41 B1 131.2(8) . . ? 
N4 N41 B1 120.8(7) . . ? 
C53 N5 N51 107.4(8) . . ? 
C53 N5 Cu 137.1(7) . . ? 
N51 N5 Cu 115.2(6) . . ? 
C51 N51 N5 107.7(8) . . ? 
C51 N51 B1 133.9(8) . . ? 
N5 N51 B1 118.2(7) . . ? 
N1 C11 C12 110.2(9) . . ? 
C11 C12 C13 105.5(9) . . ? 
N11 C13 C12 109.3(7) . . ? 
N11 C13 C14 122.0(9) . . ? 
C12 C13 C14 128.7(9) . . ? 
C13 C14 C15 113.8(8) . . ? 
C13 C14 C19 112.0(7) . . ? 
C15 C14 C19 110.2(8) . . ? 
C16 C15 C14 112.6(8) . . ? 
C17 C16 C15 112.1(8) . . ? 
C18 C17 C16 112.4(9) . . ? 
C17 C18 C19 110.6(9) . . ? 
C14 C19 C18 112.3(8) . . ? 
N2 C21 C22 110.8(9) . . ? 
C21 C22 C23 106.0(9) . . ? 
N21 C23 C22 108.0(8) . . ? 
N21 C23 C24 122.3(8) . . ? 
C22 C23 C24 129.6(9) . . ? 
C25 C24 C23 111.0(9) . . ? 
C25 C24 C29 108.6(11) . . ? 
C23 C24 C29 114.8(8) . . ? 
C24 C25 C26 112.2(11) . . ? 
C27 C26 C25 107.5(11) . . ? 
C28 C27 C26 111.2(11) . . ? 
C27 C28 C29 109.2(12) . . ? 
C24 C29 C28 112.3(9) . . ? 
N31 C31 C32 110.9(9) . . ? 
C31 C32 C33 106.2(10) . . ? 
N3 C33 C32 107.3(9) . . ? 
N3 C33 C34 120.5(8) . . ? 
C32 C33 C34 132.2(10) . . ? 
C33 C34 C39 115.4(8) . . ? 
C33 C34 C35 109.5(7) . . ? 
C39 C34 C35 109.2(8) . . ? 
C34 C35 C36 112.9(9) . . ? 
C37 C36 C35 111.2(9) . . ? 
C38 C37 C36 110.9(9) . . ? 
C37 C38 C39 113.0(9) . . ? 
C34 C39 C38 111.0(8) . . ? 
N41 C41 C42 109.5(8) . . ? 
C41 C42 C43 106.1(9) . . ? 
N4 C43 C42 108.5(8) . . ? 
N4 C43 C44 121.0(8) . . ? 
C42 C43 C44 130.2(9) . . ? 
C43 C44 C45 114.3(8) . . ? 
C43 C44 C49 110.5(8) . . ? 
C45 C44 C49 109.0(8) . . ? 
C46 C45 C44 111.0(8) . . ? 
C47 C46 C45 112.9(9) . . ? 
C46 C47 C48 110.7(10) . . ? 
C47 C48 C49 111.0(8) . . ? 
C48 C49 C44 112.0(8) . . ? 
N51 C51 C52 111.0(9) . . ? 
C51 C52 C53 105.0(9) . . ? 
N5 C53 C52 108.8(9) . . ? 
N5 C53 C54 120.4(9) . . ? 
C52 C53 C54 130.7(10) . . ? 
C53 C54 C55 110.8(8) . . ? 
C53 C54 C59 111.4(9) . . ? 
C55 C54 C59 110.9(8) . . ? 
C54 C55 C56 110.6(8) . . ? 
C57 C56 C55 111.8(10) . . ? 
C56 C57 C58 109.7(10) . . ? 
C57 C58 C59 113.6(9) . . ? 
C54 C59 C58 109.6(9) . . ? 
N41 B1 N51 110.4(8) . . ? 
N41 B1 N31 107.5(7) . . ? 
N51 B1 N31 109.9(7) . . ? 
  
_diffrn_measured_fraction_theta_max    1.000 
_diffrn_reflns_theta_full              23.00 
_diffrn_measured_fraction_theta_full   1.000 
_refine_diff_density_max    0.421 
_refine_diff_density_min   -0.407 
_refine_diff_density_rms    0.070