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_7043576
_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 Ni P2, 2(C H Cl3)'
_chemical_formula_sum            'C32 H34 B Cl8 N3 Ni P2'
_chemical_formula_weight         875.68
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-05-17
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-06-30 deposited with the CCDC.
2017-07-03 downloaded from the CCDC.
;
_cell_angle_alpha                90.040(5)
_cell_angle_beta                 103.664(5)
_cell_angle_gamma                106.259(5)
_cell_formula_units_Z            2
_cell_length_a                   9.9895(10)
_cell_length_b                   12.2230(12)
_cell_length_c                   16.8174(17)
_cell_measurement_reflns_used    9965
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      27.41
_cell_measurement_theta_min      2.45
_cell_volume                     1910.6(3)
_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 0.999
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker Nonius Kappa APEX II'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            44643
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.670
_diffrn_reflns_theta_min         2.777
_exptl_absorpt_coefficient_mu    1.180
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6803
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0503 before and 0.0398 after correction. The Ratio of minimum to maximum transmission is 0.9124. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            Orange-yellow
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular prism-like'
_exptl_crystal_F_000             892
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.867
_refine_diff_density_min         -0.715
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         8797
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0318
_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^)+(0.0350P)^2^+1.3985P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0743
_refine_ls_wR_factor_ref         0.0823
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7097
_reflns_number_total             8797
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02144e2.cif
_cod_data_source_block           dal1551
_cod_database_code               7043576
_shelx_estimated_absorpt_t_max   0.862
_shelx_estimated_absorpt_t_min   0.834
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Others
 Sof(Cl63)=Sof(Cl64)=Sof(H61A)=1-FVAR(1)
 Sof(Cl65)=Sof(Cl62)=Sof(H61)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C51(H51), C61(H61), C61(H61A)
3.b 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.c 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              32331
_olex2_submission_special_instructions 'No special instructions were received'