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_7049177
_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 H34 B F Mo N3 O4 P2, C H2 Cl2, B F4'
_chemical_formula_sum            'C35 H36 B2 Cl2 F5 Mo N3 O4 P2'
_chemical_formula_weight         908.07
_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
_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                90
_cell_angle_beta                 107.133(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.655(2)
_cell_length_b                   11.0271(11)
_cell_length_c                   17.7885(18)
_cell_measurement_reflns_used    7142
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      21.86
_cell_measurement_theta_min      2.20
_cell_volume                     3871.8(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 0.997
_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  0.0651
_diffrn_reflns_av_unetI/netI     0.0562
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            44334
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.381
_diffrn_reflns_theta_min         1.032
_exptl_absorpt_coefficient_mu    0.626
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6680
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0624 before and 0.0552 after correction. The Ratio of minimum to maximum transmission is 0.8962. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.558
_exptl_crystal_description       plate
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   0.7454
_exptl_transmission_factor_min   0.6680
_refine_diff_density_max         2.361
_refine_diff_density_min         -1.177
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         7909
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.1076
_refine_ls_R_factor_gt           0.0733
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0761P)^2^+21.5744P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1755
_refine_ls_wR_factor_ref         0.1983
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5671
_reflns_number_total             7909
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00733d3.cif
_cod_data_source_block           dal1875
_cod_depositor_comments
'Adding full bibliography for 7049175--7049178.cif.'
_cod_database_code               7049177
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.969
_shelx_estimated_absorpt_t_min   0.901
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H2(0.048) H32(0.051) H16(0.041) H36(0.049) H26(0.061) H15(0.056)
 H33(0.063) H45(0.06) H35(0.061) H46(0.051) H34(0.061) H12(0.058) H6A(0.059)
 H6B(0.059) H44(0.067) H13(0.073) H24(0.083) H14(0.065) H43(0.072) H25(0.082)
 H22(0.065) H42(0.061) H23(0.08) H5A(0.084) H5B(0.084) H2A(0.084) H2B(0.084)
 H51A(0.094) H51B(0.094) H3A(0.085) H3B(0.085) H4A(0.087) H4B(0.087) H1A(0.079)
 H1B(0.079)
 Fixed X: H2(0.2143) H32(0.4487) H16(0.3184) H36(0.2509) H3(0.1116)
 H26(0.1974) H15(0.383) H33(0.4787) H45(0.4671) H35(0.2815) H46(0.3968)
 H34(0.3943) H12(0.2783) H6A(0.2739) H6B(0.2704) H44(0.4893) H13(0.3418)
 H24(0.0426) H14(0.3932) H43(0.4549) H25(0.1111) H22(0.1407) H42(0.3845)
 H23(0.0556) H5A(0.1546) H5B(0.1842) H2A(0.0563) H2B(0.0639) H51A(0.0588)
 H51B(0.0678) H3A(0.0487) H3B(0.1158) H4A(0.1635) H4B(0.0946) H1A(0.1465)
 H1B(0.175)
 Fixed Y: H2(0.4609) H32(0.5354) H16(-0.0813) H36(0.595) H3(0.4148) H26(-
 0.1257) H15(-0.2177) H33(0.6982) H45(0.5831) H35(0.7596) H46(0.5943)
 H34(0.8115) H12(0.1026) H6A(0.5573) H6B(0.6292) H44(0.398) H13(-0.0386) H24(-
 0.1258) H14(-0.1987) H43(0.2216) H25(-0.2301) H22(0.1847) H42(0.2286)
 H23(0.0826) H5A(0.6206) H5B(0.6895) H2A(0.1462) H2B(0.2127) H51A(0.7028)
 H51B(0.5589) H3A(0.3555) H3B(0.3063) H4A(0.5189) H4B(0.5595) H1A(0.0608)
 H1B(0.1333)
 Fixed Z: H2(0.5012) H32(0.5441) H16(0.5088) H36(0.4286) H3(0.5345)
 H26(0.4975) H15(0.5998) H33(0.4762) H45(0.7852) H35(0.3646) H46(0.6564)
 H34(0.3867) H12(0.6854) H6A(0.6528) H6B(0.5735) H44(0.8483) H13(0.7751)
 H24(0.2949) H14(0.7317) H43(0.7794) H25(0.4044) H22(0.3759) H42(0.6513)
 H23(0.2838) H5A(0.5365) H5B(0.6184) H2A(0.6016) H2B(0.5245) H51A(0.2099)
 H51B(0.2098) H3A(0.6168) H3B(0.6802) H4A(0.687) H4B(0.6226) H1A(0.57)
 H1B(0.651)
;
_shelx_res_checksum              1933
_olex2_submission_special_instructions 'No special instructions were received'