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_7043580
_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         'C18 H40 B N3 P2'
_chemical_formula_sum            'C18 H40 B N3 P2'
_chemical_formula_weight         371.28
_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                 101.400(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.6254(9)
_cell_length_b                   15.2128(15)
_cell_length_c                   17.6220(18)
_cell_measurement_reflns_used    9921
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      25.79
_cell_measurement_theta_min      2.36
_cell_volume                     2266.7(4)
_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 0.998
_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  0.0499
_diffrn_reflns_av_unetI/netI     0.0343
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            52481
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.942
_diffrn_reflns_theta_min         2.926
_exptl_absorpt_coefficient_mu    0.197
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7110
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0598 before and 0.0535 after correction.
The Ratio of minimum to maximum transmission is 0.9536.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.088
_exptl_crystal_description       'irregular prism-like'
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.399
_refine_diff_density_min         -0.265
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         5424
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0369
_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^)+(0.0463P)^2^+0.6963P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0890
_refine_ls_wR_factor_ref         0.0998
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4130
_reflns_number_total             5424
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02144e2.cif
_cod_data_source_block           dal1611
_cod_database_code               7043580
_shelx_estimated_absorpt_t_max   0.982
_shelx_estimated_absorpt_t_min   0.938
_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:
 C11(H11), C21(H21), C31(H31), C41(H41)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C2(H2A,H2B), C6(H6A,H6B), C1(H1A,H1B), C5(H5A,H5B)
2.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C12(H12A,H12B,H12C), C23(H23A,H23B,H23C), C43(H43A,H43B,
 H43C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C22(H22A,H22B,H22C), C42(H42A,
 H42B,H42C)
;
_shelx_res_checksum              31089
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'