Triaminoborane-bridged diphosphine complexes with Ni and Pd: coordination chemistry, structures, and ligand-centered reactivity
Lee, Kyounghoon; Donahue, Courtney M.; Daly, Scott R.; Dalton Trans.  (2017) –; doi:10.1039/C7DT02144E

data_7043584
_publ_section_title
;
 Triaminoborane-bridged diphosphine complexes with Ni and Pd: coordination
 chemistry, structures, and ligand-centered reactivity
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02144E
_journal_year                    2017
_chemical_formula_moiety         'C30 H32 B Cl2 N3 P2 Pd'
_chemical_formula_sum            'C30 H32 B Cl2 N3 P2 Pd'
_chemical_formula_weight         684.63
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-10-17
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2017-06-30 deposited with the CCDC.
2017-07-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.019(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9178(13)
_cell_length_b                   13.3011(13)
_cell_length_c                   18.1092(18)
_cell_measurement_reflns_used    9728
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      29.03
_cell_measurement_theta_min      2.233
_cell_volume                     3018.9(5)
_computing_cell_refinement       'APEX II (Bruker-AXS, 2015)'
_computing_data_collection       'APEX II (Bruker-AXS, 2015)'
_computing_data_reduction        'APEX II (Bruker-AXS, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      190.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Nonius Kappa Apex II'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_unetI/netI     0.0150
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            74406
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.037
_diffrn_reflns_theta_min         2.922
_exptl_absorpt_coefficient_mu    0.923
_exptl_absorpt_correction_T_max  0.889
_exptl_absorpt_correction_T_min  0.820
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_description       plate
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.13
_exptl_transmission_factor_max   0.889
_exptl_transmission_factor_min   0.820
_refine_diff_density_max         0.439
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         8050
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0233
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0153P)^2^+3.4172P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0508
_refine_ls_wR_factor_ref         0.0558
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7220
_reflns_number_total             8050
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02144e2.cif
_cod_data_source_block           dal1543
_cod_database_code               7043584
_shelx_estimated_absorpt_t_max   0.889
_shelx_estimated_absorpt_t_min   0.744
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C3(H4a,H4b), C6(H1a,H1b), C4(H3a,H3b), C2(H5a,H5b), C1(H6a,H6b), C5(H2a,H2b)
2.b Aromatic/amide H refined with riding coordinates:
 C32(H16), C42(H26), C46(H22), C16(H42), C33(H15), C43(H25), C12(H46),
 C36(H12), C26(H32), C34(H14), C15(H43), C44(H24), C25(H33), C14(H44), C22(H36),
  C35(H13), C13(H45), C45(H23), C24(H34), C23(H35)
;
_shelx_res_checksum              44349
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'