Isolation of ligand-centered borocations in molybdenum complexes containing a triaminoborane-bridged diphosphorus ligand.
Lee, Kyounghoon; Kim, Chan Woo; Buckley, Jimmy L.; Vlaisavljevich, Bess; Daly, Scott R.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 3777–3785; doi:10.1039/c9dt00733d

data_7049175
_publ_section_title
;
 Isolation of ligand-centered borocations in molybdenum complexes
 containing a triaminoborane-bridged diphosphorus ligand.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3777
_journal_page_last               3785
_journal_paper_doi               10.1039/c9dt00733d
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C34 H32 B Mo N3 O4 P2'
_chemical_formula_sum            'C34 H32 B Mo N3 O4 P2'
_chemical_formula_weight         715.31
_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     dual
_audit_creation_date             2018-12-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-12-20 deposited with the CCDC.    2019-02-20 downloaded from the CCDC.
;
_cell_angle_alpha                84.673(5)
_cell_angle_beta                 85.261(5)
_cell_angle_gamma                84.632(5)
_cell_formula_units_Z            4
_cell_length_a                   10.3852(10)
_cell_length_b                   15.1206(15)
_cell_length_c                   20.549(2)
_cell_measurement_reflns_used    71814
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      26.02
_cell_measurement_theta_min      1.00
_cell_volume                     3189.9(5)
_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 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Nonius Kappa APEX II'
_diffrn_measurement_method       'CCD phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_unetI/netI     0.0478
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            23407
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.050
_diffrn_reflns_theta_min         1.358
_exptl_absorpt_coefficient_mu    0.555
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_description       plate
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   0.7454
_exptl_transmission_factor_min   0.6147
_refine_diff_density_max         0.988
_refine_diff_density_min         -0.442
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     811
_refine_ls_number_reflns         12584
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_gt           0.0343
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0304P)^2^+2.2553P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0711
_refine_ls_wR_factor_ref         0.0787
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9594
_reflns_number_total             12584
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00733d3.cif
_cod_data_source_block           dal1753
_cod_depositor_comments
'Adding full bibliography for 7049175--7049178.cif.'
_cod_database_code               7049175
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.967
_shelx_estimated_absorpt_t_min   0.842
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H45(0.038) H92(0.034) H4A(0.036) H4B(0.036) H36(0.029) H12(0.033)
 H44(0.04) H14(0.045) H82(0.036) H93(0.041) H46(0.032) H33(0.039) H3A(0.04)
 H3B(0.04) H35(0.035) H43(0.04) H13(0.041) H72(0.036) H42(0.034) H65A(0.038)
 H65B(0.038) H5A(0.037) H5B(0.037) H61A(0.034) H61B(0.034) H94(0.049)
 H6A(0.035) H6B(0.035) H73(0.046) H16(0.037) H106(0.038) H26(0.036) H66A(0.036)
 H66B(0.036) H96(0.038) H32(0.031) H34(0.041) H105(0.052) H15(0.045)
 H63A(0.044) H63B(0.044) H74(0.048) H64A(0.04) H64B(0.04) H62A(0.04) H62B(0.04)
 H104(0.054) H95(0.047) H102(0.04) H83(0.049) H25(0.051) H85(0.048) H86(0.037)
 H76(0.041) H22(0.041) H24(0.059) H103(0.049) H75(0.049) H1A(0.048) H1B(0.048)
 H84(0.052) H23(0.056) H2A(0.055) H2B(0.055)
 Fixed X: H45(0.5862) H92(0.6087) H4A(0.5581) H4B(0.4335) H36(0.3108)
 H12(0.4003) H44(0.8085) H14(0.6518) H82(0.6345) H93(0.3896) H46(0.4847)
 H33(0.2605) H3A(0.3402) H3B(0.4804) H35(0.1039) H43(0.9299) H13(0.456)
 H72(0.8726) H42(0.8305) H65A(0.6945) H65B(0.7724) H5A(0.608) H5B(0.6914)
 H61A(0.8396) H61B(0.7468) H94(0.3272) H6A(0.4624) H6B(0.6068) H73(1.0072)
 H16(0.7421) H106(0.7387) H26(0.4883) H66A(0.7692) H66B(0.9143) H96(0.7032)
 H32(0.4667) H34(0.0789) H105(0.8094) H15(0.7953) H63A(0.8443) H63B(0.9967)
 H74(1.2172) H64A(0.9573) H64B(0.8365) H62A(1.0193) H62B(0.9107) H104(1.0108)
 H95(0.4834) H102(1.0773) H83(0.4342) H25(0.3176) H85(0.6144) H86(0.8148)
 H76(1.1615) H22(0.2511) H24(0.1151) H103(1.1448) H75(1.2936) H1A(0.2767)
 H1B(0.339) H84(0.4243) H23(0.0826) H2A(0.4876) H2B(0.341)
 Fixed Y: H45(1.1792) H92(0.8463) H4A(0.7527) H4B(0.8178) H36(0.8765)
 H12(0.4813) H44(1.1758) H14(0.2839) H82(0.6726) H93(0.864) H46(1.0476)
 H33(0.9602) H3A(0.6697) H3B(0.6205) H35(0.9143) H43(1.0393) H13(0.3302)
 H72(0.4647) H42(0.9072) H65A(0.8154) H65B(0.879) H5A(0.9025) H5B(0.8265)
 H61A(0.516) H61B(0.5701) H94(0.9053) H6A(0.9244) H6B(0.9444) H73(0.3331)
 H16(0.5394) H106(1.0459) H26(0.5809) H66A(0.9278) H66B(0.9047) H96(0.919)
 H32(0.9179) H34(0.9555) H105(1.1865) H15(0.3884) H63A(0.5863) H63B(0.5967)
 H74(0.3281) H64A(0.7767) H64B(0.7269) H62A(0.5294) H62B(0.4744) H104(1.1996)
 H95(0.9296) H102(0.932) H83(0.6593) H25(0.5796) H85(0.5657) H86(0.5842)
 H76(0.5899) H22(0.7191) H24(0.6479) H103(1.0719) H75(0.4573) H1A(0.6611)
 H1B(0.5775) H84(0.6052) H23(0.7196) H2A(0.5445) H2B(0.5395)
 Fixed Z: H45(0.6238) H92(0.24) H4A(0.9117) H4B(0.8929) H36(0.7139)
 H12(0.6343) H44(0.6325) H14(0.7069) H82(0.1842) H93(0.2203) H46(0.6317)
 H33(0.4925) H3A(0.8831) H3B(0.8958) H35(0.6776) H43(0.6496) H13(0.6622)
 H72(0.0955) H42(0.6564) H65A(0.3501) H65B(0.3879) H5A(0.8726) H5B(0.8339)
 H61A(0.2204) H61B(0.2722) H94(0.1146) H6A(0.7876) H6B(0.7601) H73(0.0964)
 H16(0.6941) H106(0.1328) H26(0.5228) H66A(0.275) H66B(0.2959) H96(0.0489)
 H32(0.5276) H34(0.5673) H105(0.1397) H15(0.7217) H63A(0.3876) H63B(0.3774)
 H74(0.1293) H64A(0.3835) H64B(0.4179) H62A(0.2833) H62B(0.3246) H104(0.1781)
 H95(0.0288) H102(0.1974) H83(0.1437) H25(0.4568) H85(-0.0199) H86(0.0173)
 H76(0.1564) H22(0.651) H24(0.4866) H103(0.2062) H75(0.1596) H1A(0.7623)
 H1B(0.7244) H84(0.0425) H23(0.5825) H2A(0.8041) H2B(0.8343)
;
_shelx_res_checksum              677
_olex2_submission_special_instructions 'No special instructions were received'