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_7718581
_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         'C43 H74 B O Os P2, C2 F6 N O4 S2, C H2 Cl2'
_chemical_formula_sum            'C46 H76 B Cl2 F6 N O5 Os P2 S2'
_chemical_formula_weight         1235.04
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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                 94.936(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.850(4)
_cell_length_b                   18.960(5)
_cell_length_c                   16.990(4)
_cell_measurement_reflns_used    9879
_cell_measurement_temperature    120.00
_cell_measurement_theta_max      29.99
_cell_measurement_theta_min      2.41
_cell_volume                     5408(2)
_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 5.6
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 6000 area detector'
_diffrn_measurement_method       '\w 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  0.0900
_diffrn_reflns_av_unetI/netI     0.0435
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            98977
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.406
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_target            Mo
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    2.657
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.5202
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dull light orange'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_description       block
_exptl_crystal_F_000             2520
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.580
_refine_diff_density_min         -1.230
_refine_diff_density_rms         0.109
_refine_ls_extinction_coef       0.00031(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     692
_refine_ls_number_reflns         9513
_refine_ls_number_restraints     379
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0364
_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^)+(0.0398P)^2^+16.3303P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0931
_refine_ls_wR_factor_ref         0.0963
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8174
_reflns_number_total             9513
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00777a2.cif
_cod_data_source_block           mo_22may01tmh2_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'None' was changed
to 'none' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7718580--7718581.cif.
;
_cod_database_code               7718581
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.777
_shelx_estimated_absorpt_t_min   0.646
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 F2-C2
 1.3 with sigma of 0.01
 Os1-H3
 1.58 with sigma of 0.01
 C56-C55 \\sim C56-C55A
 with sigma of 0.02
 C54-C55 \\sim C55A-C54
 with sigma of 0.02
 C55-C54 \\sim C55A-C54
 with sigma of 0.02
 C55-C56 \\sim C55A-C56
 with sigma of 0.02
 C53-C52 \\sim C53-C52A
 with sigma of 0.02
 C52A-C51 \\sim C52-C51
 with sigma of 0.02
 C52-C53 \\sim C52A-C53
 with sigma of 0.02
 C51-C52 \\sim C51-C52A
 with sigma of 0.02
 F6-C3 \\sim F6A-C3A
 with sigma of 0.02
 F4-C3 \\sim F4A-C3A
 with sigma of 0.02
 O4-S2 \\sim O4A-S2A
 with sigma of 0.02
 N1-S2 \\sim N1-S2A
 with sigma of 0.02
 F5-C3 \\sim F5A-C3A
 with sigma of 0.02
 O5-S2 \\sim O5A-S2A
 with sigma of 0.02
 C3-S2 \\sim C3A-S2A
 with sigma of 0.02
 F6-F4 \\sim F6A-F4A
 with sigma of 0.04
 F6-F5 \\sim F6A-F5A
 with sigma of 0.04
 F6-S2 \\sim F6A-S2A
 with sigma of 0.04
 F4-F5 \\sim F4A-F5A
 with sigma of 0.04
 F4-S2 \\sim F4A-S2A
 with sigma of 0.04
 O4-N1 \\sim O4A-N1
 with sigma of 0.04
 O4-O5 \\sim O4A-O5A
 with sigma of 0.04
 O4-C3 \\sim O4A-C3A
 with sigma of 0.04
 N1-O5 \\sim N1-O5A
 with sigma of 0.04
 N1-C3 \\sim N1-C3A
 with sigma of 0.04
 F5-S2 \\sim F5A-S2A
 with sigma of 0.04
 O5-C3 \\sim O5A-C3A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
S1 \\sim S2 \\sim S2A \\sim O1 \\sim O3 \\sim O2 \\sim O4 \\sim O5 \\sim O4A
\\sim O5A \\sim F1 \\sim F6 \\sim F4 \\sim F2 \\sim F5 \\sim F3 \\sim F4A \\sim
F5A \\sim F6A \\sim N1 \\sim C2 \\sim C3 \\sim C3A: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(F1) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F5) \\sim
Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 C11, C16, C15, C14, C13, C12
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 O4, S2, O5, F4, C3, F6, F5
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5. Others
 Sof(H01O)=Sof(H01P)=Sof(HL)=Sof(HM)=Sof(C55A)=Sof(H1A)=Sof(H1B)=1-FVAR(1)
 Sof(H56A)=Sof(H56B)=Sof(C55)=Sof(H55A)=Sof(H55B)=Sof(H54A)=Sof(H54B)=FVAR(1)
 Sof(H01U)=Sof(H01V)=Sof(H01X)=Sof(C52A)=Sof(H11)=Sof(HP)=1-FVAR(2)
 Sof(H53A)=Sof(H53B)=Sof(H51)=Sof(C52)=Sof(H52A)=Sof(H52B)=FVAR(2)
 Sof(O4A)=Sof(S2A)=Sof(O5A)=Sof(F4A)=Sof(C3A)=Sof(F5A)=Sof(F6A)=1-FVAR(3)
 Sof(F6)=Sof(F4)=Sof(O4)=Sof(F5)=Sof(O5)=Sof(C3)=Sof(S2)=FVAR(3)
6.a Ternary CH refined with riding coordinates:
 C31(H31), C41(H41), C21(H21), C61(H61), C71(H71), C51(H51), C51(H01X)
6.b Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C25(H25A,H25B), C46(H46A,H46B), C32(H32A,H32B), C43(H43A,
 H43B), C62(H62A,H62B), C22(H22A,H22B), C72(H72A,H72B), C66(H66A,H66B),
 C42(H42A,H42B), C76(H76A,H76B), C73(H73A,H73B), C36(H00A,H00B), C24(H24A,H24B),
  C45(H45A,H45B), C65(H65A,H65B), C35(H35A,H35B), C64(H64A,H64B), C23(H23A,
 H23B), C33(H33A,H33B), C44(H44A,H44B), C63(H63A,H63B), C56(H56A,H56B),
 C56(H01O,H01P), C75(H75A,H75B), C53(H53A,H53B), C53(H01U,H01V), C74(H74A,H74B),
  C34(H34A,H34B), C52(H52A,H52B), C55(H55A,H55B), C54(H54A,H54B), C54(HL,HM),
 C4(H01A,H01B), C55A(H1A,H1B), C52A(H11,HP)
6.c Aromatic/amide H refined with riding coordinates:
 C16(H16), C12(H12), C15(H15), C13(H13), C14(H14)
;
_shelx_res_checksum              87239
_shelx_hkl_checksum              51013
_olex2_submission_special_instructions 'No special instructions were received'