Expanding the allyl analogy: accessing η<sup>3</sup>-P,B,P diphosphinoborane complexes of group 10.
Drover, Marcus W.; Peters, Jonas C.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 3733–3738; doi:10.1039/c8dt00058a

data_7045537
_publ_section_title
;
 Expanding the allyl analogy: accessing \h<sup>3</sup>-P,B,P
 diphosphinoborane complexes of group 10.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3733
_journal_page_last               3738
_journal_paper_doi               10.1039/c8dt00058a
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C43 H39 B N2 Ni P2'
_chemical_formula_sum            'C43 H39 B N2 Ni P2'
_chemical_formula_weight         715.22
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2017-10-23
_audit_creation_method
;
Olex2 1.2
(compiled Aug 10 2017 17:28:52 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-10-23 deposited with the CCDC.
2018-02-05 downloaded from the CCDC.
;
_cell_angle_alpha                110.291(5)
_cell_angle_beta                 98.272(6)
_cell_angle_gamma                94.867(6)
_cell_formula_units_Z            2
_cell_length_a                   11.0162(11)
_cell_length_b                   13.4010(14)
_cell_length_c                   16.5488(17)
_cell_measurement_reflns_used    9378
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.427
_cell_measurement_theta_min      2.461
_cell_volume                     2243.6(4)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'Bruker AXS D8 Venture Kappa'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0782
_diffrn_reflns_av_unetI/netI     0.0781
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            45938
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.814
_diffrn_reflns_theta_min         1.637
_exptl_absorpt_coefficient_mu    0.531
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6197
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1021 before and 0.0762 after correction. The Ratio of minimum to maximum transmission is 0.8309. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.059
_exptl_crystal_description       block
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.024
_refine_diff_density_min         -1.364
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         12328
_refine_ls_number_restraints     435
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.0868
_refine_ls_R_factor_gt           0.0658
_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^)+(0.1261P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1757
_refine_ls_wR_factor_ref         0.1902
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9094
_reflns_number_total             12328
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00058a2.cif
_cod_data_source_block           a17027_0m
_cod_depositor_comments
'Adding full bibliography for 7045536--7045541.cif.'
_cod_database_code               7045537
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.939
_shelx_estimated_absorpt_t_min   0.888
_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. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Aromatic/amide H refined with riding coordinates:
 C33(H33), C18(H18), C41(H41), C22(H22), C25(H25), C43(H43), C16(H16),
 C12(H12), C42(H42), C2(H2), C15(H15), C27(H27), C5(H5), C37(H37), C19(H19),
 C20(H20), C40(H40), C36(H36), C21(H21), C34(H34), C39(H39), C13(H13), C10(H10),
  C35(H35), C14(H14), C3(H3), C4(H4), C7(H7), C9(H9), C8(H8)
3.b Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C)
;
_olex2_submission_special_instructions 'No special instructions were received'