Reactions of nickel boranyl compounds with pnictogen-carbon triple bonds.
Austen, Brady J. H.; Clapson, Marissa L.; Drover, Marcus W.; RSC advances 13 (2023) 19158–19163; doi:10.1039/d3ra02797j

data_7246947
_publ_section_title
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 Reactions of nickel boranyl compounds with pnictogen-carbon triple bonds.
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_journal_issue                   28
_journal_name_full               'RSC advances'
_journal_page_first              19158
_journal_page_last               19163
_journal_paper_doi               10.1039/d3ra02797j
_journal_volume                  13
_journal_year                    2023
_chemical_formula_moiety         'C42 H81 B2 N Ni P2, C7 H8'
_chemical_formula_sum            'C49 H89 B2 N Ni P2'
_chemical_formula_weight         834.48
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-12-16
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-03-22 deposited with the CCDC.	2023-06-14 downloaded from the CCDC.
;
_cell_angle_alpha                67.397(5)
_cell_angle_beta                 68.276(5)
_cell_angle_gamma                78.741(5)
_cell_formula_units_Z            2
_cell_length_a                   13.2771(17)
_cell_length_b                   13.8480(18)
_cell_length_c                   15.682(2)
_cell_measurement_reflns_used    9315
_cell_measurement_temperature    170.0
_cell_measurement_theta_max      28.35
_cell_measurement_theta_min      2.23
_cell_volume                     2468.1(6)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      170.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0511
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_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       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            159104
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.400
_diffrn_reflns_theta_min         1.985
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.490
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6837
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1102 before and 0.0565 after correction.
The Ratio of minimum to maximum transmission is 0.9169.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.123
_exptl_crystal_description       block
_exptl_crystal_F_000             916
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.034
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     504
_refine_ls_number_reflns         12337
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0419
_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^)+(0.0624P)^2^+1.5743P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1124
_refine_ls_wR_factor_ref         0.1260
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10550
_reflns_number_total             12337
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ra02797j2.cif
_cod_data_source_block           final11
_cod_original_cell_volume        2468.0(6)
_cod_database_code               7246947
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.976
_shelx_estimated_absorpt_t_min   0.953
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1), C7(H7), C29(H29), C35(H35)
2.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C26(H26A,H26B), C14(H14A,H14B), C15(H15A,H15B), C27(H27A,
 H27B), C8(H8A,H8B), C12(H12A,H12B), C2(H2A,H2B), C20(H20A,H20B), C6(H6A,H6B),
 C11(H11A,H11B), C28(H28A,H28B), C21(H21A,H21B), C34(H34A,H34B), C10(H10A,H10B),
  C36(H36A,H36B), C5(H5A,H5B), C3(H3A,H3B), C9(H9A,H9B), C4(H4A,H4B), C33(H33A,
 H33B), C30(H30A,H30B), C40(H40A,H40B), C32(H32A,H32B), C37(H37A,H37B),
 C31(H31A,H31B), C38(H38A,H38B), C39(H39A,H39B)
2.c Aromatic/amide H refined with riding coordinates:
 C49(H49), C43(H43), C46(H46), C44(H44), C45(H45)
2.d Idealised Me refined as rotating group:
 C48(H48A,H48B,H48C), C18(H18A,H18B,H18C), C25(H25A,H25B,H25C), C19(H19A,H19B,
 H19C), C17(H17A,H17B,H17C), C24(H24A,H24B,H24C), C23(H23A,H23B,H23C), C41(H41A,
 H41B,H41C)
;
_shelx_res_checksum              27725
_olex2_submission_special_instructions 'No special instructions were received'