Crystal structure of dichlorido(N-o-tolyl-1,1-di-p-tolylphosphanamine–κ1 P)-(methoxydi-p-tolylphosphane-κ1 P)palladium(II), C36H39Cl2NOP2Pd
Kama, Dumisani V.; Brink, Alice; Roodt, Andreas; Zeitschrift für Kristallographie - New Crystal Structures 235 (2020) 349–352; doi:10.1515/ncrs-2019-0659

data_8105104
_publ_section_title
;
 Crystal structure of
 dichlorido(N-o-tolyl-1,1-di-p-tolylphosphanamine--\k1
 P)-(methoxydi-p-tolylphosphane-\k1 P)palladium(II), C36H39Cl2NOP2Pd
;
_journal_issue                   2
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              349
_journal_page_last               352
_journal_paper_doi               10.1515/ncrs-2019-0659
_journal_volume                  235
_journal_year                    2020
_chemical_formula_moiety         'C36 H39 Cl2 N O P2 Pd'
_chemical_formula_sum            'C36 H39 Cl2 N O P2 Pd'
_chemical_formula_weight         740.92
_chemical_name_systematic
;
dichloro[1,1-di-<i>p</i>-tolyl-<i>N</i>-(2-methylbenzene)
phosphinamide-<i>k</i>P](methyl-di-<i>p</i>-
tolylphosphinite-<i>k</i>P)-palladium(II)
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.209(13)
_cell_length_b                   15.144(11)
_cell_length_c                   24.011(19)
_cell_measurement_reflns_used    9967
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      2.51
_cell_volume                     6985(9)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012) [1]'
_computing_data_collection       'Bruker, Apex2 [1]'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012) [1]'
_computing_molecular_graphics    'Diamond 3.2 [4]'
_computing_publication_material  'Olex2-2009 [5]'
_computing_structure_refinement  'SHELXL-2018/3 [3]'
_computing_structure_solution    'SHELXT-2018/2 [2]'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0676
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            135723
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         27.998
_diffrn_reflns_theta_min         2.820
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.805
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5413
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1591 before and 0.0670 after correction.
The Ratio of minimum to maximum transmission is 0.7259.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_description       Plate
_exptl_crystal_F_000             3040
_exptl_crystal_size_max          0.87
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.078
_refine_diff_density_max         0.475
_refine_diff_density_min         -0.560
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         8414
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0292
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0316P)^2^+4.0319P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0706
_refine_ls_wR_factor_ref         0.0867
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6389
_reflns_number_total             8414
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2019-0659_suppl.cif
_cod_data_source_block           exp_1115
_cod_database_code               8105104
_shelx_estimated_absorpt_t_min   0.541
_shelx_estimated_absorpt_t_max   0.940
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C5(H5), C4(H4), C3(H3), C12(H12), C13(H13), C15(H15), C16(H16),
 C22(H22), C23(H23), C25(H25), C26(H26), C32(H32), C33(H33), C35(H35), C36(H36),
  C42(H42), C43(H43), C45(H45), C46(H46)
2.b Fitted hexagon refined as free rotating group:
 C2(C1,C6,C5,C4,C3)
2.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C17(H17A,H17B,H17C), C27(H27A,H27B,H27C),
 C37(H37A,H37B,H37C), C47(H47A,H47B,H47C)
;