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_7043582
_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
'C60 H68 B2 F2 N6 Ni2 O2 P4, 2(Cl), 2(C H2 Cl2)'
_chemical_formula_sum            'C62 H72 B2 Cl6 F2 N6 Ni2 O2 P4'
_chemical_formula_weight         1446.87
_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             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
_cell_angle_beta                 91.629(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3721(12)
_cell_length_b                   32.375(3)
_cell_length_c                   16.7696(17)
_cell_measurement_reflns_used    9675
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      27.81
_cell_measurement_theta_min      2.25
_cell_volume                     6714.3(11)
_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 0.984
_diffrn_measurement_device_type  'Bruker Nonius Kappa APEX II'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            107878
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.926
_diffrn_reflns_theta_min         2.764
_exptl_absorpt_coefficient_mu    0.948
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7087
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0510 before and 0.0408 after correction. The Ratio of minimum to maximum transmission is 0.9505. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_description       'irregular prism'
_exptl_crystal_F_000             2992
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.094
_refine_diff_density_min         -1.199
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     783
_refine_ls_number_reflns         15831
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0471
_refine_ls_R_factor_gt           0.0378
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0432P)^2^+7.3900P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0923
_refine_ls_wR_factor_ref         0.0982
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13529
_reflns_number_total             15831
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02144e2.cif
_cod_data_source_block           dal1691
_cod_database_code               7043582
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.856
_shelx_estimated_absorpt_t_min   0.703
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2.a Ternary CH refined with riding coordinates:
 N3(H3), N6(H6)
2.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C3(H3A,H3B), C4(H4A,H4B), C6(H6A,H6B), C1(H1A,H1B), C51(H51A,
 H51B), C52(H52A,H52B), C2(H2A,H2B), C56(H56A,H56B), C54(H54A,H54B), C55(H55A,
 H55B), C53(H53A,H53B), C102(H10C,H10D), C101(H10A,H10B)
2.c Aromatic/amide H refined with riding coordinates:
 C62(H62), C66(H66), C72(H72), C65(H65), C36(H36), C64(H64), C96(H96),
 C63(H63), C73(H73), C76(H76), C75(H75), C42(H42), C95(H95), C46(H46), C12(H12),
  C32(H32), C74(H74), C92(H92), C33(H33), C43(H43), C94(H94), C34(H34),
 C26(H26), C45(H45), C35(H35), C82(H82), C24(H24), C86(H86), C16(H16), C13(H13),
  C44(H44), C93(H93), C22(H22), C25(H25), C83(H83), C23(H23), C14(H14),
 C84(H84), C15(H15), C85(H85)
;
_shelx_res_checksum              54252
_olex2_submission_special_instructions 'No special instructions were received'