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_7049178
_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, C2 F6 N O4 S2, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C36.5 H34 B Cl F6 Mo N4 O8 P2 S2'
_chemical_formula_weight         1038.93
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   mixed
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.741(2)
_cell_length_b                   9.9649(10)
_cell_length_c                   44.148(4)
_cell_measurement_reflns_used    9829
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      22.19
_cell_measurement_theta_min      2.26
_cell_volume                     8684.7(15)
_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 0.998
_diffrn_measured_fraction_theta_max 0.993
_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  0.0795
_diffrn_reflns_av_unetI/netI     0.0595
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -55
_diffrn_reflns_number            120089
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.429
_diffrn_reflns_theta_min         2.063
_exptl_absorpt_coefficient_mu    0.613
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6653
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0757 before and 0.0691 after correction. The Ratio of minimum to maximum transmission is 0.8925. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_description       plate
_exptl_crystal_F_000             4200
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   0.7545
_exptl_transmission_factor_min   0.6653
_refine_diff_density_max         1.297
_refine_diff_density_min         -1.483
_refine_diff_density_rms         0.104
_refine_ls_abs_structure_details
;
 Flack x determined using 6232 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.036(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1116
_refine_ls_number_reflns         17717
_refine_ls_number_restraints     80
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0547
_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^)+(0.0159P)^2^+27.4604P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0985
_refine_ls_wR_factor_ref         0.1024
_reflns_Friedel_coverage         0.968
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                15465
_reflns_number_total             17717
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00733d3.cif
_cod_data_source_block           dal1841
_cod_depositor_comments
'Adding full bibliography for 7049175--7049178.cif.'
_cod_original_cell_volume        8684.6(15)
_cod_original_formula_sum        'C36.50 H34 B Cl F6 Mo N4 O8 P2 S2'
_cod_database_code               7049178
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.976
_shelx_estimated_absorpt_t_min   0.842
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H1A(0.021) H1B(0.021) H2A(0.026) H2B(0.026) H3A(0.025) H3B(0.025)
 H4A(0.03) H4B(0.03) H5A(0.032) H5B(0.032) H6A(0.022) H6B(0.022) H6(0.016)
 H16(0.022) H25(0.036) H33(0.024) H56A(0.026) H56B(0.026) H55A(0.028)
 H55B(0.028) H32(0.025) H12(0.036) H73(0.041) H35(0.028) H86(0.024) H96(0.031)
 H26(0.026) H83(0.03) H84(0.026) H24(0.032) H42(0.03) H95(0.033) H13(0.048)
 H76(0.03) H93(0.048) H54A(0.025) H54B(0.025) H53A(0.027) H53B(0.027) H66(0.03)
 H34(0.028) H45(0.039) H72(0.035) H15(0.032) H62(0.026) H74(0.043) H63(0.044)
 H64(0.049) H65(0.047) H82(0.023) H85(0.029) H52A(0.026) H52B(0.026) H94(0.047)
 H46(0.025) H22(0.023) H23(0.032) H36(0.026) H75(0.042) H92(0.035) H44(0.048)
 H43(0.049) H14(0.052) H51A(0.028) H51B(0.028) H10A(0.094) H10B(0.094)
 H10C(0.094) H10D(0.094)
 Fixed X: H1A(0.4338) H1B(0.4456) H2A(0.3754) H2B(0.4194) H3A(0.4382)
 H3B(0.4701) H4A(0.5902) H4B(0.5482) H5A(0.6237) H5B(0.6738) H6A(0.7006)
 H6B(0.626) H6(0.6469) H16(0.5264) H25(0.3683) H33(0.8696) H56A(0.8281)
 H56B(0.7539) H55A(0.7994) H55B(0.7526) H32(0.8213) H12(0.5961) H73(0.562)
 H35(0.7391) H86(0.8174) H96(0.9704) H26(0.4556) H83(0.9943) H84(0.9527)
 H24(0.3579) H42(0.6734) H95(1.0316) H13(0.5972) H76(0.5943) H93(0.8622)
 H54A(0.6705) H54B(0.7108) H53A(0.5915) H53B(0.5613) H66(0.6514) H34(0.8267)
 H45(0.9028) H72(0.6423) H15(0.5305) H62(0.727) H74(0.5013) H63(0.7295)
 H64(0.7024) H65(0.6577) H82(0.948) H85(0.8624) H52A(0.5505) H52B(0.5005)
 H94(0.9775) H46(0.8436) H22(0.5236) H23(0.4338) H36(0.6903) H75(0.517)
 H92(0.8003) H44(0.8478) H43(0.734) H14(0.5629) H51A(0.5605) H51B(0.5695)
 H10A(0.9466) H10B(0.8736) H10C(0.875) H10D(0.834)
 Fixed Y: H1A(0.4477) H1B(0.3007) H2A(0.403) H2B(0.5383) H3A(0.4033)
 H3B(0.2895) H4A(0.3143) H4B(0.3974) H5A(0.5621) H5B(0.4429) H6A(0.5939)
 H6B(0.6567) H6(0.9434) H16(0.6711) H25(0.3735) H33(0.3831) H56A(0.9126)
 H56B(0.8481) H55A(1.0629) H55B(0.9388) H32(0.4924) H12(0.5304) H73(1.4998)
 H35(0.0761) H86(1.3267) H96(1.0242) H26(0.4882) H83(1.1262) H84(1.3329)
 H24(0.1409) H42(0.7189) H95(0.8351) H13(0.7485) H76(1.0488) H93(0.6121)
 H54A(1.0938) H54B(1.1876) H53A(1.2072) H53B(1.0875) H66(0.841) H34(0.1779)
 H45(0.6765) H72(1.3746) H15(0.8901) H62(0.988) H74(1.3987) H63(0.7761)
 H64(0.5905) H65(0.6255) H82(1.017) H85(1.4326) H52A(0.9552) H52B(1.082)
 H94(0.6313) H46(0.4895) H22(0.1345) H23(0.0237) H36(0.1849) H75(1.1739)
 H92(0.8007) H44(0.8807) H43(0.901) H14(0.9273) H51A(1.0603) H51B(1.2043)
 H10A(0.7925) H10B(0.7408) H10C(0.7447) H10D(0.6217)
 Fixed Z: H1A(0.3977) H1B(0.3843) H2A(0.3505) H2B(0.3505) H3A(0.3062)
 H3B(0.3277) H4A(0.3063) H4B(0.2815) H5A(0.2797) H5B(0.2893) H6A(0.3249)
 H6B(0.3256) H6(0.6801) H16(0.3939) H25(0.4839) H33(0.2914) H56A(0.6764)
 H56B(0.6752) H55A(0.712) H55B(0.7218) H32(0.3331) H12(0.4738) H73(0.5583)
 H35(0.302) H86(0.6587) H96(0.6158) H26(0.4588) H83(0.7121) H84(0.7273)
 H24(0.4789) H42(0.3802) H95(0.6015) H13(0.4934) H76(0.5354) H93(0.6031)
 H54A(0.7206) H54B(0.6973) H53A(0.6746) H53B(0.695) H66(0.6057) H34(0.2749)
 H45(0.4042) H72(0.5853) H15(0.413) H62(0.5274) H74(0.5194) H63(0.5076)
 H64(0.5374) H65(0.5865) H82(0.6698) H85(0.7009) H52A(0.6487) H52B(0.6497)
 H94(0.5947) H46(0.3872) H22(0.4261) H23(0.449) H36(0.3433) H75(0.5086)
 H92(0.6197) H44(0.4104) H43(0.3979) H14(0.463) H51A(0.6023) H51B(0.6178)
 H10A(0.5225) H10B(0.533) H10C(0.5329) H10D(0.5187)
;
_shelx_res_checksum              13734
_olex2_submission_special_instructions 'No special instructions were received'