Facile synthesis of air-stable heterobimetallic osmium-silver hydride complexes.
Zhou, Haiyu; Bai, Tongtong; Pan, Yanlin; Wei, Yongliang; Wang, Tongdao; Dalton transactions (Cambridge, England : 2003) 50 (2021) 12093–12097; doi:10.1039/d1dt02619d

data_7708061
_publ_section_title
;
 Facile synthesis of air-stable heterobimetallic osmium-silver hydride
 complexes.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12093
_journal_page_last               12097
_journal_paper_doi               10.1039/d1dt02619d
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C65 H56 Ag O Os P3'
_chemical_formula_sum            'C65 H56 Ag O Os P3'
_chemical_formula_weight         1244.07
_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     iterative
_audit_creation_date             2021-02-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-08-13 deposited with the CCDC.	2021-08-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.0280(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1963(4)
_cell_length_b                   29.4703(10)
_cell_length_c                   13.9338(4)
_cell_measurement_reflns_used    9519
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.444
_cell_measurement_theta_min      2.437
_cell_volume                     5378.1(3)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      120.15
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX2 microsource'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_unetI/netI     0.0182
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            125506
_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         27.522
_diffrn_reflns_theta_min         2.372
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    2.856
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6182
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0652 before and 0.0455 after correction.
The Ratio of minimum to maximum transmission is 0.8291.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_description       block
_exptl_crystal_F_000             2488
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.814
_refine_diff_density_min         -0.797
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     689
_refine_ls_number_reflns         12348
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0379
_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^)+(0.0426P)^2^+23.7083P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0947
_refine_ls_wR_factor_ref         0.1004
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11039
_reflns_number_total             12348
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02619d2.cif
_cod_data_source_block           mo_19nov8btta_0m_pl
_cod_depositor_comments
'Adding full bibliography for 7708061--7708062.cif.'
_cod_database_code               7708061
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.599
_shelx_estimated_absorpt_t_min   0.366
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 P2-C21A \\sim P2-C211
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C24A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C21A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 C211, C212, C213, C214, C215, C216
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(C26A)=Sof(H26A)=Sof(C21A)=Sof(C22A)=Sof(H22A)=Sof(C23A)=Sof(H23A)=
 Sof(C24A)=Sof(H24A)=Sof(C25A)=Sof(H25A)=1-FVAR(1)
 Sof(C211)=Sof(C212)=Sof(H212)=Sof(C213)=Sof(H213)=Sof(C214)=Sof(H214)=
 Sof(C215)=Sof(H215)=Sof(C216)=Sof(H216)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C26A(H26A), C22A(H22A), C23A(H23A), C24A(H24A), C25A(H25A), C102(H102),
 C103(H103), C104(H104), C105(H105), C106(H106), C112(H112), C113(H113),
 C114(H114), C115(H115), C116(H116), C122(H122), C123(H123), C124(H124),
 C125(H125), C126(H126), C202(H202), C203(H203), C204(H204), C205(H205),
 C206(H206), C212(H212), C213(H213), C214(H214), C215(H215), C216(H216),
 C222(H222), C223(H223), C224(H224), C225(H225), C226(H226), C302(H302),
 C303(H303), C304(H304), C305(H305), C306(H306), C312(H312), C313(H313),
 C314(H314), C315(H315), C316(H316), C322(H322), C323(H323), C324(H324),
 C325(H325), C326(H326)
6.b Fitted hexagon refined as free rotating group:
 C26A(C21A,C22A,C23A,C24A,C25A)
6.c X=CH2 refined with riding coordinates:
 C4(H4A,H4B), C9(H9A,H9B)
6.d Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              72473
_olex2_submission_special_instructions 'No special instructions were received'