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_7043577
_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 H35 B N3 Ni O2 P2, Cl'
_chemical_formula_sum            'C30 H35 B Cl N3 Ni O2 P2'
_chemical_formula_weight         636.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-10-04
_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                 106.374(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8071(14)
_cell_length_b                   11.3545(11)
_cell_length_c                   20.486(2)
_cell_measurement_reflns_used    10298
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      1.00
_cell_volume                     3081.4(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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      190.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Nonius Kappa Apex II'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0616
_diffrn_reflns_av_unetI/netI     0.0541
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            20425
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.378
_diffrn_reflns_theta_max         25.378
_diffrn_reflns_theta_min         2.741
_exptl_absorpt_coefficient_mu    0.852
_exptl_absorpt_correction_T_max  0.9749
_exptl_absorpt_correction_T_min  0.8281
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.290
_refine_diff_density_min         -0.340
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.881
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         5637
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.881
_refine_ls_R_factor_all          0.0718
_refine_ls_R_factor_gt           0.0391
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1073
_refine_ls_wR_factor_ref         0.1320
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4011
_reflns_number_total             5637
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02144e2.cif
_cod_data_source_block           dal1630
_cod_database_code               7043577
_shelx_estimated_absorpt_t_max   0.975
_shelx_estimated_absorpt_t_min   0.828
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 O1-H1 = O2-H2
 0.85 with sigma of 0.01
 N3-H3
 0.93 with sigma of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B)
3.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C22(H22), C23(H23),
 C24(H24), C25(H25), C26(H26), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36),
  C42(H42), C43(H43), C44(H44), C45(H45), C46(H46)
;
_shelx_res_checksum              41855
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'