# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mr_ps_bdy_cho_autored
_database_code_depnum_ccdc_archive 'CCDC 2128295'
loop_
_audit_author_name
_audit_author_address
'Kamakshya Nath panda'
;indian institute of technology bombay
India
;
_audit_update_record             
;
2021-12-13 deposited with the CCDC.	2022-03-09 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_RINTA01_mr_ps_bdy_cho_autored 
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: We tried to get better crystal, but for all the crystallographic parameters were similar.
;
# Added during the CSD deposition process: Monday 13 December 2021 06:01 PM
# end Validation Reply Form

_audit_creation_date             2021-12-13
_audit_creation_method           
;
Olex2 1.2-ac3
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_chemical_formula_moiety         'C21 H16 B F2 N3 O'
_chemical_formula_sum            'C21 H16 B F2 N3 O'
_chemical_formula_weight         375.20
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
C 0.00347 0.00161 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
B 0.00141 0.00067 2.05450 1.33260 1.09790 0.70680 23.21850 1.02100 60.34980
0.14030 -0.193200007081
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
F 0.01794 0.01033 3.53920 2.64120 1.51700 1.02430 10.28250 4.29440 0.26150
26.14760 0.277599990368
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
O 0.01158 0.00611 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390
32.90890 0.250800013542
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.00653 0.00323 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.5290002823
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 x+1/2,-y+1/2,-z
3 -x,y+1/2,-z+1/2
4 -x+1/2,-y,z+1/2
5 -x,-y,-z
6 -x-1/2,y-1/2,z
7 x,-y-1/2,z-1/2
8 x-1/2,y,-z-1/2

_symmetry_Int_Tables_number      61
_cell_length_a                   10.1997(8)
_cell_length_b                   15.3185(11)
_cell_length_c                   22.490(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3513.9(5)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    877
_cell_measurement_temperature    105(7)
_cell_measurement_theta_max      18.6520
_cell_measurement_theta_min      2.6570
_exptl_absorpt_coefficient_mu    0.103
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81024
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark pink'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.4183
_exptl_crystal_description       plate
_exptl_crystal_F_000             1552.8330
_exptl_crystal_size_max          0.154
_exptl_crystal_size_mid          0.121
_exptl_crystal_size_min          0.091
_diffrn_reflns_av_R_equivalents  0.2034
_diffrn_reflns_av_unetI/netI     0.2269
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            33811
_diffrn_reflns_theta_full        24.9999
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.66
_diffrn_ambient_temperature      105.15
_diffrn_measured_fraction_theta_full 0.9984
_diffrn_measured_fraction_theta_max 0.9984
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ     75.79 204.29   0.50    5.00  15.81  -9.84 -59.25    --   257
  2  ω   -100.81  15.69   0.50    5.00    --   -9.84 -59.25  20.08  233
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              0
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                1999
_reflns_number_total             3093
_reflns_threshold_expression     I>=2u(I)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_refine_diff_density_max         0.4076
_refine_diff_density_min         -0.4693
_refine_diff_density_rms         0.1107
_refine_ls_d_res_high            0.8409
_refine_ls_d_res_low             7.6593
_refine_ls_goodness_of_fit_ref   1.0400
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    30
_refine_ls_number_parameters     254
_refine_ls_number_reflns         3093
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0986
_refine_ls_R_factor_gt           0.0560
_refine_ls_restrained_S_all      1.0400
_refine_ls_shift/su_max          0.0005
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0521P)²+1.3720P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1210
_refine_ls_wR_factor_ref         0.1457
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C20(H20), C14(H14), C12(H12), C3(H3), C8(H8), C4(H4), C7(H7),
 C19(H19), C17(H17), C16(H16), C1(H1a), C13(H13)
2.b Idealised Me refined as rotating group:
 C21(H21b,H21c,H21a)
;
_atom_sites_solution_primary     direct
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_refinement_flags_posn
F1 F 0.23562(15) 0.27792(11) 0.61533(8) 0.0271(5) Uani 1.000000 .
F2 F 0.21074(15) 0.42428(11) 0.62368(8) 0.0283(5) Uani 1.000000 .
O1 O 0.4435(2) 0.28726(15) 0.77716(11) 0.0346(6) Uani 1.000000 .
N1 N 0.4753(2) 0.34125(16) 0.65535(11) 0.0229(6) Uani 1.000000 .
H1 H 0.3978(2) 0.31678(16) 0.65953(11) 0.0274(7) Uiso 1.000000 R
N2 N 0.3252(2) 0.36966(15) 0.53731(11) 0.0190(6) Uani 1.000000 .
N3 N 0.0853(2) 0.34877(15) 0.54898(12) 0.0217(6) Uani 1.000000 .
C1 C 0.5447(3) 0.3200(2) 0.75918(15) 0.0285(8) Uani 1.000000 .
H1a H 0.6144(3) 0.3260(2) 0.78686(15) 0.0342(9) Uiso 1.000000 R
C2 C 0.5674(3) 0.35013(19) 0.70002(14) 0.0241(7) Uani 1.000000 .
C3 C 0.6747(3) 0.39318(19) 0.67571(15) 0.0242(7) Uani 1.000000 .
H3 H 0.7529(3) 0.40871(19) 0.69604(15) 0.0290(9) Uiso 1.000000 R
C4 C 0.6469(3) 0.40929(19) 0.61664(15) 0.0239(7) Uani 1.000000 .
H4 H 0.7029(3) 0.43813(19) 0.58919(15) 0.0286(9) Uiso 1.000000 R
C5 C 0.5223(3) 0.37595(19) 0.60405(14) 0.0213(7) Uani 1.000000 .
C6 C 0.4563(3) 0.37892(18) 0.54710(14) 0.0210(7) Uani 1.000000 .
C7 C 0.5196(3) 0.39539(19) 0.49281(14) 0.0244(8) Uani 1.000000 .
H7 H 0.6111(3) 0.40360(19) 0.48729(14) 0.0292(9) Uiso 1.000000 R
C8 C 0.4259(3) 0.39751(19) 0.44924(14) 0.0229(7) Uani 1.000000 .
H8 H 0.4405(3) 0.40817(19) 0.40816(14) 0.0274(9) Uiso 1.000000 R
C9 C 0.3039(3) 0.38103(18) 0.47630(14) 0.0207(7) Uani 1.000000 .
C10 C 0.1776(3) 0.37567(18) 0.45099(14) 0.0209(7) Uani 1.000000 .
C11 C 0.0694(3) 0.35755(19) 0.48791(14) 0.0207(7) Uani 1.000000 .
C12 C -0.0624(3) 0.34099(19) 0.47433(15) 0.0246(7) Uani 1.000000 .
H12 H -0.1009(3) 0.34170(19) 0.43587(15) 0.0295(9) Uiso 1.000000 R
C13 C -0.1257(3) 0.3235(2) 0.52710(15) 0.0265(8) Uani 1.000000 .
H13 H -0.2162(3) 0.3105(2) 0.53170(15) 0.0318(9) Uiso 1.000000 R
C14 C -0.0328(3) 0.32834(19) 0.57262(15) 0.0241(7) Uani 1.000000 .
H14 H -0.0497(3) 0.31881(19) 0.61365(15) 0.0289(9) Uiso 1.000000 R
C15 C 0.1574(3) 0.38845(18) 0.38703(14) 0.0204(7) Uani 1.000000 .
C16 C 0.2356(3) 0.3461(2) 0.34449(15) 0.0249(8) Uani 1.000000 .
H16 H 0.3040(3) 0.3085(2) 0.35726(15) 0.0299(9) Uiso 1.000000 R
C17 C 0.2146(3) 0.35835(19) 0.28428(15) 0.0253(7) Uani 1.000000 .
H17 H 0.2691(3) 0.32926(19) 0.25635(15) 0.0303(9) Uiso 1.000000 R
C18 C 0.1144(3) 0.41280(19) 0.26403(15) 0.0242(7) Uani 1.000000 .
C19 C 0.0361(3) 0.4543(2) 0.30586(15) 0.0249(7) Uani 1.000000 .
H19 H -0.0331(3) 0.4912(2) 0.29280(15) 0.0299(9) Uiso 1.000000 R
C20 C 0.0566(3) 0.44298(18) 0.36624(15) 0.0231(7) Uani 1.000000 .
H20 H 0.0019(3) 0.47244(18) 0.39392(15) 0.0277(9) Uiso 1.000000 R
C21 C 0.0918(3) 0.4247(2) 0.19850(16) 0.0339(9) Uani 1.000000 .
H21b H 0.1595(12) 0.4632(11) 0.1821(2) 0.0508(13) Uiso 1.000000 GR
H21c H 0.0959(19) 0.3679(3) 0.1786(2) 0.0508(13) Uiso 1.000000 GR
H21a H 0.0053(9) 0.4508(12) 0.19203(16) 0.0508(13) Uiso 1.000000 GR
B1 B 0.2144(3) 0.3555(2) 0.58357(16) 0.0209(8) Uani 1.000000 .


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
F1 B1 1.403(4) . ?
F2 B1 1.388(4) . ?
O1 C1 1.216(4) . ?
N1 C2 1.382(4) . ?
N1 C5 1.358(4) . ?
N2 C6 1.363(4) . ?
N2 C9 1.400(4) . ?
N2 B1 1.551(4) . ?
N3 C11 1.390(4) . ?
N3 C14 1.353(4) . ?
N3 B1 1.533(4) . ?
C1 C2 1.427(4) . ?
C2 C3 1.389(4) . ?
C3 C4 1.381(4) . ?
C4 C5 1.398(4) . ?
C5 C6 1.447(4) . ?
C6 C7 1.404(4) . ?
C7 C8 1.369(4) . ?
C8 C9 1.408(4) . ?
C9 C10 1.411(4) . ?
C10 C11 1.409(4) . ?
C10 C15 1.466(4) . ?
C11 C12 1.401(4) . ?
C12 C13 1.377(4) . ?
C13 C14 1.398(4) . ?
C15 C16 1.404(4) . ?
C15 C20 1.405(4) . ?
C16 C17 1.384(4) . ?
C17 C18 1.395(4) . ?
C18 C19 1.388(4) . ?
C18 C21 1.503(5) . ?
C19 C20 1.385(4) . ?

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
C5 N1 C2 109.8(2) . . ?
C9 N2 C6 107.3(2) . . ?
B1 N2 C6 128.4(3) . . ?
B1 N2 C9 124.2(2) . . ?
C14 N3 C11 107.9(2) . . ?
B1 N3 C11 126.5(2) . . ?
B1 N3 C14 125.5(3) . . ?
C2 C1 O1 125.5(3) . . ?
C1 C2 N1 122.3(3) . . ?
C3 C2 N1 107.2(3) . . ?
C3 C2 C1 130.4(3) . . ?
C4 C3 C2 107.6(3) . . ?
C5 C4 C3 108.4(3) . . ?
C4 C5 N1 107.0(3) . . ?
C6 C5 N1 126.9(3) . . ?
C6 C5 C4 126.2(3) . . ?
C5 C6 N2 126.6(3) . . ?
C7 C6 N2 109.2(3) . . ?
C7 C6 C5 124.2(3) . . ?
C8 C7 C6 107.8(3) . . ?
C9 C8 C7 107.7(3) . . ?
C8 C9 N2 108.0(2) . . ?
C10 C9 N2 122.0(3) . . ?
C10 C9 C8 130.0(3) . . ?
C11 C10 C9 119.3(3) . . ?
C15 C10 C9 121.1(3) . . ?
C15 C10 C11 119.7(3) . . ?
C10 C11 N3 120.7(3) . . ?
C12 C11 N3 108.1(3) . . ?
C12 C11 C10 131.2(3) . . ?
C13 C12 C11 107.3(3) . . ?
C14 C13 C12 107.6(3) . . ?
C13 C14 N3 109.2(3) . . ?
C16 C15 C10 121.8(3) . . ?
C20 C15 C10 120.6(3) . . ?
C20 C15 C16 117.6(3) . . ?
C17 C16 C15 121.1(3) . . ?
C18 C17 C16 120.9(3) . . ?
C19 C18 C17 118.3(3) . . ?
C21 C18 C17 120.3(3) . . ?
C21 C18 C19 121.4(3) . . ?
C20 C19 C18 121.3(3) . . ?
C19 C20 C15 120.8(3) . . ?
F2 B1 F1 108.4(3) . . ?
N2 B1 F1 110.3(2) . . ?
N2 B1 F2 110.5(2) . . ?
N3 B1 F1 109.5(2) . . ?
N3 B1 F2 111.0(2) . . ?
N3 B1 N2 107.1(3) . . ?


_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_fastscan_autored
_database_code_depnum_ccdc_archive 'CCDC 2128296'
loop_
_audit_author_name
_audit_author_address
'Kamakshya Nath panda'
;indian institute of technology bombay
India
;
_audit_update_record             
;
2021-12-13 deposited with the CCDC.	2022-03-09 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H17 N3 O2 Pd'
_chemical_formula_weight         449.77
_chemical_absolute_configuration ?
_chemical_melting_point          ?
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'
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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   7.2123(4)
_cell_length_b                   8.5123(5)
_cell_length_c                   29.3664(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1802.90(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    10282
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.02
_cell_measurement_theta_min      2.49
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.051
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4861
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.657
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0698
_diffrn_reflns_av_unetI/netI     0.0722
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            10282
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.024
_diffrn_reflns_theta_max         25.024
_diffrn_reflns_theta_min         2.491
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'Omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_reflns_Friedel_coverage         0.703
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                2913
_reflns_number_total             3171
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_refine_diff_density_max         1.998
_refine_diff_density_min         -1.133
_refine_diff_density_rms         0.213
_refine_ls_abs_structure_details 
;
 Flack x determined using 945 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.01(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         3171
_refine_ls_number_restraints     303
_refine_ls_R_factor_all          0.0972
_refine_ls_R_factor_gt           0.0910
_refine_ls_restrained_S_all      1.113
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1098P)²+23.8633P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2385
_refine_ls_wR_factor_ref         0.2450
_refine_special_details          ?
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.40300(18) 0.48435(16) 0.41978(4) 0.0319(4) Uani 1 1 d . U . . .
O1 O 0.785(2) 0.6462(17) 0.4898(5) 0.046(4) Uani 1 1 d . U . . .
O2 O 0.4766(19) 0.6965(17) 0.4481(5) 0.038(3) Uani 1 1 d G U . . .
H1 H 0.5803 0.6751 0.4619 0.057 Uiso 1 1 d G U . . .
H2 H 0.3939 0.6965 0.4696 0.057 Uiso 1 1 d G U . . .
N1 N 0.6303(19) 0.3591(17) 0.4403(5) 0.027(3) Uani 1 1 d . U . . .
N2 N 0.344(2) 0.285(2) 0.3925(6) 0.043(4) Uani 1 1 d . U . . .
N3 N 0.166(2) 0.568(3) 0.3943(6) 0.052(4) Uani 1 1 d . U . . .
C1 C 0.858(2) 0.516(2) 0.4858(6) 0.037(4) Uani 1 1 d . U . . .
H3 H 0.9771 0.5076 0.4994 0.044 Uiso 1 1 calc R U . . .
C2 C 0.794(2) 0.377(2) 0.4639(6) 0.029(3) Uani 1 1 d . U . . .
C3 C 0.894(3) 0.237(2) 0.4637(6) 0.035(4) Uani 1 1 d . U . . .
H4 H 1.0141 0.2198 0.4758 0.042 Uiso 1 1 calc R U . . .
C4 C 0.782(3) 0.126(2) 0.4421(7) 0.038(4) Uani 1 1 d . U . . .
H5 H 0.8064 0.0173 0.4382 0.046 Uiso 1 1 calc R U . . .
C5 C 0.628(2) 0.207(2) 0.4277(6) 0.033(3) Uani 1 1 d . U . . .
C6 C 0.468(3) 0.167(3) 0.4003(7) 0.041(4) Uani 1 1 d . U . . .
C7 C 0.408(3) 0.029(3) 0.3766(8) 0.059(5) Uani 1 1 d . U . . .
H6 H 0.4631 -0.0721 0.3769 0.070 Uiso 1 1 calc R U . . .
C8 C 0.248(3) 0.076(3) 0.3527(8) 0.057(5) Uani 1 1 d . U . . .
H7 H 0.1784 0.0120 0.3326 0.068 Uiso 1 1 calc R U . . .
C9 C 0.208(3) 0.235(3) 0.3632(7) 0.047(4) Uani 1 1 d . U . . .
C10 C 0.069(3) 0.333(4) 0.3481(8) 0.061(5) Uani 1 1 d . U . . .
C11 C 0.050(3) 0.479(4) 0.3638(7) 0.061(5) Uani 1 1 d . U . . .
C12 C -0.096(5) 0.597(4) 0.3536(10) 0.091(7) Uani 1 1 d . U . . .
H8 H -0.1956 0.5801 0.3330 0.109 Uiso 1 1 calc R U . . .
C13 C -0.071(4) 0.729(4) 0.3764(10) 0.083(7) Uani 1 1 d . U . . .
H9 H -0.1477 0.8200 0.3756 0.099 Uiso 1 1 calc R U . . .
C14 C 0.082(4) 0.711(4) 0.4007(8) 0.066(6) Uani 1 1 d . U . . .
H10 H 0.1299 0.7891 0.4207 0.079 Uiso 1 1 calc R U . . .
C15 C -0.053(3) 0.239(3) 0.3147(5) 0.073(6) Uani 1 1 d G U . . .
C16 C -0.168(3) 0.112(3) 0.3250(6) 0.102(10) Uani 1 1 d G U . . .
H11 H -0.1634 0.0660 0.3544 0.123 Uiso 1 1 calc R U . . .
C17 C -0.290(3) 0.054(3) 0.2924(7) 0.110(10) Uani 1 1 d G U . . .
H12 H -0.3681 -0.0318 0.2995 0.131 Uiso 1 1 calc R U . . .
C18 C -0.296(3) 0.122(3) 0.2494(6) 0.099(9) Uani 1 1 d G U . . .
C19 C -0.181(3) 0.249(2) 0.2390(5) 0.074(8) Uani 1 1 d G U . . .
H16 H -0.1859 0.2950 0.2096 0.089 Uiso 1 1 calc R U . . .
C20 C -0.060(3) 0.307(2) 0.2717(6) 0.081(8) Uani 1 1 d G U . . .
H17 H 0.0187 0.3929 0.2646 0.097 Uiso 1 1 calc R U . . .
C21 C -0.468(5) 0.101(6) 0.2150(12) 0.116(12) Uani 1 1 d . U . . .
H13 H -0.5611 0.0319 0.2288 0.173 Uiso 1 1 calc R U . . .
H14 H -0.5240 0.2038 0.2087 0.173 Uiso 1 1 calc R U . . .
H15 H -0.4243 0.0545 0.1864 0.173 Uiso 1 1 calc R U . . .


_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
Pd1 O2 2.058(15) . ?
Pd1 N1 2.047(14) . ?
Pd1 N2 1.924(19) . ?
Pd1 N3 1.998(18) . ?
O1 C1 1.23(2) . ?
N1 C2 1.37(2) . ?
N1 C5 1.35(2) . ?
N2 C6 1.36(3) . ?
N2 C9 1.38(3) . ?
N3 C11 1.44(3) . ?
N3 C14 1.37(3) . ?
C2 C1 1.42(3) . ?
C2 C3 1.40(3) . ?
C3 C4 1.39(3) . ?
C5 C4 1.37(3) . ?
C5 C6 1.45(3) . ?
C7 C6 1.43(3) . ?
C7 C8 1.41(3) . ?
C8 C9 1.41(4) . ?
C9 C10 1.37(3) . ?
C11 C10 1.34(4) . ?
C11 C12 1.49(4) . ?
C12 C13 1.32(4) . ?
C14 C13 1.33(4) . ?
C15 C10 1.55(3) . ?
C15 C16 1.3900 . ?
C15 C20 1.3900 . ?
C17 C16 1.3900 . ?
C18 C17 1.3900 . ?
C18 C21 1.61(4) . ?
C19 C18 1.3900 . ?
C20 C19 1.3900 . ?

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 Pd1 O2 97.5(6) . . ?
N2 Pd1 O2 177.7(6) . . ?
N2 Pd1 N1 80.8(7) . . ?
N2 Pd1 N3 88.3(8) . . ?
N3 Pd1 O2 93.4(7) . . ?
N3 Pd1 N1 169.1(8) . . ?
C2 N1 Pd1 140.9(12) . . ?
C5 N1 Pd1 114.1(11) . . ?
C5 N1 C2 105.1(15) . . ?
C6 N2 Pd1 115.8(13) . . ?
C6 N2 C9 110.1(19) . . ?
C9 N2 Pd1 134.0(17) . . ?
C11 N3 Pd1 122.9(17) . . ?
C14 N3 Pd1 129.9(18) . . ?
C14 N3 C11 107(2) . . ?
O1 C1 C2 130.5(17) . . ?
N1 C2 C1 126.9(16) . . ?
N1 C2 C3 110.0(16) . . ?
C3 C2 C1 123.1(17) . . ?
C4 C3 C2 106.4(18) . . ?
C5 C4 C3 105.6(18) . . ?
N1 C5 C4 112.7(17) . . ?
N1 C5 C6 113.0(17) . . ?
C4 C5 C6 134.2(18) . . ?
N2 C6 C5 116.2(18) . . ?
N2 C6 C7 108.8(19) . . ?
C7 C6 C5 135(2) . . ?
C8 C7 C6 105(2) . . ?
C7 C8 C9 109(2) . . ?
N2 C9 C8 107(2) . . ?
C10 C9 N2 122(2) . . ?
C10 C9 C8 131(2) . . ?
C9 C10 C15 108(2) . . ?
C11 C10 C9 122(2) . . ?
C11 C10 C15 130(2) . . ?
N3 C11 C12 100(3) . . ?
C10 C11 N3 130(2) . . ?
C10 C11 C12 130(2) . . ?
C13 C12 C11 112(3) . . ?
C12 C13 C14 107(3) . . ?
C13 C14 N3 113(3) . . ?
C16 C15 C10 127.0(15) . . ?
C20 C15 C10 112.4(16) . . ?
C20 C15 C16 120.0 . . ?
C17 C16 C15 120.0 . . ?
C18 C17 C16 120.0 . . ?
C17 C18 C19 120.0 . . ?
C17 C18 C21 123.4(19) . . ?
C19 C18 C21 114(2) . . ?
C18 C19 C20 120.0 . . ?
C15 C20 C19 120.0 . . ?

