Syntheses and structures of cationic osmium bis(σ-B-H) borane complexes.
Yang, Xiaowen; Tian, Minghui; Wei, Yongliang; Han, Feifei; Wang, Tongdao; Dalton transactions (Cambridge, England : 2003) 54 (2025) 9069–9075; doi:10.1039/d5dt00777a

data_7718580
_publ_section_title
;
 Syntheses and structures of cationic osmium bis(&#x3c3;-B-H) borane
 complexes.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9069
_journal_page_last               9075
_journal_paper_doi               10.1039/d5dt00777a
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C46 H80 B O Os P2, C2 F6 N O4 S2'
_chemical_formula_sum            'C48 H80 B F6 N O5 Os P2 S2'
_chemical_formula_weight         1192.20
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2025-04-01
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2025.03.04 svn.red2d20d0 for OlexSys, GUI svn.r7188)
;
_audit_update_record
;
2025-04-01 deposited with the CCDC.	2025-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.553(2)
_cell_length_b                   16.8037(18)
_cell_length_c                   19.306(2)
_cell_measurement_reflns_used    9876
_cell_measurement_temperature    120.00
_cell_measurement_theta_max      28.215
_cell_measurement_theta_min      2.433
_cell_volume                     5370.0(10)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2016)'
_computing_data_collection       'Bruker D8 Venture diffractometer'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120.00
_diffrn_detector                 'Bruker PHOTON 100 CMOS'
_diffrn_detector_area_resol_mean 7.4
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0979
_diffrn_reflns_av_unetI/netI     0.1052
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            55997
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.231
_diffrn_reflns_theta_min         2.424
_diffrn_source                   'sealed tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    2.576
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.4492
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1610 before and 0.0889 after correction.
The Ratio of minimum to maximum transmission is 0.6021.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2448
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.597
_refine_diff_density_min         -1.181
_refine_diff_density_rms         0.132
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.317(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     794
_refine_ls_number_reflns         15354
_refine_ls_number_restraints     967
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.0714
_refine_ls_R_factor_gt           0.0443
_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^)+(0.0138P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0798
_refine_ls_wR_factor_ref         0.0875
_reflns_Friedel_coverage         0.789
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.929
_reflns_number_gt                12197
_reflns_number_total             15354
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00777a2.cif
_cod_data_source_block           mo_22mar13tmh1_0m
_cod_depositor_comments
'Adding full bibliography for 7718580--7718581.cif.'
_cod_original_cell_volume        5370.0(11)
_cod_database_code               7718580
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.783
_shelx_estimated_absorpt_t_min   0.554
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.683(7)
 0.317(7)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All B(H,H) groups, All C(H,H,H) groups
3. Restrained distances
 Os1-H3
 1.58 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
P1 \\sim C41 \\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim P2 \\sim
O1 \\sim C1 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim
C17 \\sim C18 \\sim C19 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim
C26 \\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35 \\sim C36 \\sim C51 \\sim
C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C61 \\sim C62 \\sim C63 \\sim
C64 \\sim C65 \\sim C66 \\sim C71 \\sim C72 \\sim C73 \\sim C74 \\sim C75 \\sim
C76 \\sim B1 \\sim S1 \\sim S2 \\sim F1 \\sim F2 \\sim F3 \\sim F4 \\sim F5
\\sim F6 \\sim O2 \\sim O3 \\sim O4 \\sim O5 \\sim N1 \\sim C2 \\sim C3 \\sim
S1A \\sim S2A \\sim F1A \\sim F2A \\sim F3A \\sim F4A \\sim F5A \\sim F6A \\sim
O2A \\sim O3A \\sim O4A \\sim O5A \\sim N1A \\sim C2A \\sim C3A \\sim C41A
\\sim C42A \\sim C43A \\sim C44A \\sim C45A \\sim C46A: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
S1 \\sim S2 \\sim S1A \\sim S2A \\sim O1 \\sim O2 \\sim O3 \\sim O4 \\sim O5
\\sim O2A \\sim O3A \\sim O4A \\sim O5A \\sim F1 \\sim F2 \\sim F3 \\sim F4
\\sim F5 \\sim F6 \\sim F1A \\sim F2A \\sim F3A \\sim F4A \\sim F5A \\sim F6A
\\sim N1 \\sim N1A \\sim C2 \\sim C3 \\sim C2A \\sim C3A: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 2A
5. Same fragment restrains
{S1A, S2A, F1A, F2A, F3A, F4A, F5A, F6A, O2A, O3A, O4A, O5A, N1A, C2A, C3A}
sigma for 1-2: 0.01, 1-3: 0.01
as in
{S1, S2, F1, F2, F3, F4, F5, F6, O2, O3, O4, O5, N1, C2, C3}
{P1, C41A, C42A, C43A, C44A, C45A, C46A} sigma for 1-2: 0.01, 1-3: 0.01
as in
{P1, C41, C42, C43, C44, C45, C46}
6. Others
 Sof(S1A)=Sof(S2A)=Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=
 Sof(O2A)=Sof(O3A)=Sof(O4A)=Sof(O5A)=Sof(N1A)=Sof(C2A)=Sof(C3A)=1-FVAR(1)
 Sof(S1)=Sof(S2)=Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=Sof(O2)=
 Sof(O3)=Sof(O4)=Sof(O5)=Sof(N1)=Sof(C2)=Sof(C3)=FVAR(1)
 Sof(C41A)=Sof(H41A)=Sof(C42A)=Sof(H42C)=Sof(H42D)=Sof(C43A)=Sof(H43C)=
 Sof(H43D)=Sof(C44A)=Sof(H44C)=Sof(H44D)=Sof(C45A)=Sof(H45C)=Sof(H45D)=
 Sof(C46A)=Sof(H46C)=Sof(H46D)=1-FVAR(2)
 Sof(C41)=Sof(H41)=Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(C43)=Sof(H43A)=Sof(H43B)=
 Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(C46)=Sof(H46A)=
 Sof(H46B)=FVAR(2)
7.a Riding coordinates:
 B1(H2,H1)
7.b Ternary CH refined with riding coordinates:
 C41(H41), C21(H21), C31(H31), C51(H51), C61(H61), C71(H71), C41A(H41A)
7.c Secondary CH2 refined with riding coordinates:
 C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,
 H46B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B),
 C26(H26A,H26B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B),
  C36(H36A,H36B), C52(H52A,H52B), C53(H53A,H53B), C54(H54A,H54B), C55(H55A,
 H55B), C56(H56A,H56B), C62(H62A,H62B), C63(H63A,H63B), C64(H64A,H64B),
 C65(H65A,H65B), C66(H66A,H66B), C72(H72A,H72B), C73(H73A,H73B), C74(H74A,H74B),
  C75(H75A,H75B), C76(H76A,H76B), C42A(H42C,H42D), C43A(H43C,H43D), C44A(H44C,
 H44D), C45A(H45C,H45D), C46A(H46C,H46D)
7.d Aromatic/amide H refined with riding coordinates:
 C13(H13), C15(H15)
7.e Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              62039
_shelx_hkl_checksum              29549
_olex2_submission_special_instructions 'No special instructions were received'