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_7049176
_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 H33 B Mo N3 O4 P2, C F3 O3 S, C H2 Cl2'
_chemical_formula_sum            'C36 H35 B Cl2 F3 Mo N3 O7 P2 S'
_chemical_formula_weight         950.32
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-12-20
_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                90
_cell_angle_beta                 105.030(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.0807(15)
_cell_length_b                   14.2045(14)
_cell_length_c                   19.3900(19)
_cell_measurement_reflns_used    9944
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.38
_cell_measurement_theta_min      2.45
_cell_volume                     4011.5(7)
_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      150.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_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  0.0338
_diffrn_reflns_av_unetI/netI     0.0244
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            60803
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.422
_diffrn_reflns_theta_min         2.003
_exptl_absorpt_coefficient_mu    0.657
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6985
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0496 before and 0.0441 after correction. The Ratio of minimum to maximum transmission is 0.9371. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_description       lath
_exptl_crystal_F_000             1928
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   0.7454
_exptl_transmission_factor_min   0.6985
_refine_diff_density_max         0.848
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     438
_refine_ls_number_reflns         8196
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0339
_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^)+(0.0250P)^2^+7.9706P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0733
_refine_ls_wR_factor_ref         0.0807
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6826
_reflns_number_total             8196
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00733d3.cif
_cod_data_source_block           dal1865
_cod_depositor_comments
'Adding full bibliography for 7049175--7049178.cif.'
_cod_database_code               7049176
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.974
_shelx_estimated_absorpt_t_min   0.827
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H36(0.026) H35(0.032) H32(0.028) H22(0.039) H12(0.031) H34(0.036)
 H26(0.031) H13(0.042) H25(0.044) H33(0.037) H14(0.051) H24(0.054) H23(0.053)
 H15(0.054) H16(0.042) H47A(0.059) H47B(0.059) H3A(0.025) H3B(0.025) H42(0.036)
 H43(0.036) H44(0.036) H45(0.036) H46(0.036) H1A(0.025) H1B(0.025) H2A(0.025)
 H2B(0.025) H3C(0.025) H3D(0.025) H4A(0.025) H4B(0.025) H5A(0.025) H5B(0.025)
 H6A(0.025) H6B(0.025) H42A(0.036) H43A(0.036) H44A(0.036) H45A(0.036)
 H46A(0.036) H1AA(0.025) H1AB(0.025) H2AA(0.025) H2AB(0.025) H3AA(0.025)
 H3AB(0.025) H4AA(0.025) H4AB(0.025) H5AA(0.025) H5AB(0.025) H6AA(0.025)
 H6AB(0.025)
 Fixed X: H36(0.6724) H35(0.7062) H32(0.5765) H22(0.8384) H12(0.9643)
 H34(0.6678) H26(0.8243) H13(1.0675) H25(0.8836) H33(0.6079) H14(1.0217)
 H24(0.9219) H23(0.8984) H15(0.8715) H16(0.7682) H47A(1.2083) H47B(1.2279)
 H3A(0.7544) H3B(0.7818) H42(0.4579) H43(0.3004) H44(0.2034) H45(0.2639)
 H46(0.4215) H1A(0.9297) H1B(0.8949) H2A(0.9588) H2B(0.9132) H3C(0.8075)
 H3D(0.8347) H4A(0.6392) H4B(0.6729) H5A(0.569) H5B(0.5222) H6A(0.648)
 H6B(0.5427) H42A(0.4438) H43A(0.2899) H44A(0.2163) H45A(0.2967) H46A(0.4506)
 H1AA(0.9215) H1AB(0.8832) H2AA(0.9367) H2AB(0.9048) H3AA(0.8141) H3AB(0.7634)
 H4AA(0.6271) H4AB(0.6873) H5AA(0.5568) H5AB(0.6413) H6AA(0.509) H6AB(0.5243)
 Fixed Y: H36(0.3612) H35(0.5172) H32(0.445) H22(0.3371) H12(0.2203)
 H34(0.6374) H26(0.3342) H13(0.1189) H25(0.4867) H33(0.6012) H14(-0.0315)
 H24(0.5636) H23(0.4895) H15(-0.0808) H16(0.0191) H47A(0.302) H47B(0.2322)
 H3A(0.1344) H3B(0.1287) H42(0.4112) H43(0.4232) H44(0.296) H45(0.1569)
 H46(0.145) H1A(0.1632) H1B(0.0601) H2A(0.0411) H2B(0.1358) H3C(-0.0277) H3D(-
 0.0023) H4A(-0.0069) H4B(-0.0057) H5A(0.0995) H5B(0.0793) H6A(0.2292)
 H6B(0.2411) H42A(0.4088) H43A(0.3978) H44A(0.2513) H45A(0.1159) H46A(0.1269)
 H1AA(0.1806) H1AB(0.2015) H2AA(0.0521) H2AB(0.0226) H3AA(-0.0316) H3AB(-
 0.0152) H4AA(0.0096) H4AB(0.0207) H5AA(0.1131) H5AB(0.1841) H6AA(0.1342)
 H6AB(0.2374)
 Fixed Z: H36(0.3448) H35(0.3245) H32(0.5115) H22(0.4651) H12(0.6398)
 H34(0.3924) H26(0.6711) H13(0.7147) H25(0.6858) H33(0.4888) H14(0.7383)
 H24(0.5912) H23(0.4812) H15(0.6865) H16(0.6107) H47A(0.5042) H47B(0.5714)
 H3A(0.3161) H3B(0.3298) H42(0.3597) H43(0.306) H44(0.3104) H45(0.3685)
 H46(0.4223) H1A(0.5058) H1B(0.5188) H2A(0.4261) H2B(0.3876) H3C(0.403)
 H3D(0.3303) H4A(0.3509) H4B(0.2789) H5A(0.2292) H5B(0.2929) H6A(0.2887)
 H6B(0.2906) H42A(0.3669) H43A(0.3022) H44A(0.2866) H45A(0.3356) H46A(0.4003)
 H1AA(0.5045) H1AB(0.4208) H2AA(0.4201) H2AB(0.4896) H3AA(0.3647) H3AB(0.427)
 H4AA(0.3167) H4AB(0.2601) H5AA(0.2187) H5AB(0.2459) H6AA(0.3224) H6AB(0.2941)
;
_shelx_res_checksum              54630
_olex2_submission_special_instructions 'No special instructions were received'