Unsymmetric (μ-oxido)/(μ-pyrazolato) and Symmetric (μ-pyrazolato)2 Bridged Diosmium Frameworks: Electronic Structure and Magnetic Properties.
Das, Ankita; Ghosh, Prabir; Priego, José Luis; Jiménez-Aparicio, Reyes; Lahiri, Goutam Kumar; Inorganic chemistry 55 (2016) 8396–8406; doi:10.1021/acs.inorgchem.6b00898

data_4348030
_publ_section_title
;
 Unsymmetric (\m-oxido)/(\m-pyrazolato) and Symmetric (\m-pyrazolato)2
 Bridged Diosmium Frameworks: Electronic Structure and Magnetic
 Properties.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8396
_journal_page_last               8406
_journal_paper_doi               10.1021/acs.inorgchem.6b00898
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C46 H38 N12 Os2, 2(Cl O4)'
_chemical_formula_sum            'C46 H38 Cl2 N12 O8 Os2'
_chemical_formula_weight         1338.18
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-03-29
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                82.37(3)
_cell_angle_beta                 85.35(3)
_cell_angle_gamma                71.88(2)
_cell_formula_units_Z            2
_cell_length_a                   10.134(7)
_cell_length_b                   14.0076(10)
_cell_length_c                   16.941(12)
_cell_measurement_reflns_used    3550
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.57
_cell_measurement_theta_min      2.98
_cell_volume                     2263(2)
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b28'
_computing_data_collection       'CrystalClear-SM Expert 2.1 b28 (Rigaku, 2013)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b28'
_computing_molecular_graphics    ORTEP
_computing_publication_material  ORTEP
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0929
_diffrn_reflns_av_unetI/netI     0.0797
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            31491
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.241
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.020
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    5.797
_exptl_absorpt_correction_T_max  0.4238
_exptl_absorpt_correction_T_min  0.4238
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.964
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         4.589
_refine_diff_density_min         -2.999
_refine_diff_density_rms         0.267
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         7960
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.0704
_refine_ls_R_factor_gt           0.0624
_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^)+(0.0603P)^2^+26.2988P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1460
_refine_ls_wR_factor_ref         0.1567
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7094
_reflns_number_total             7960
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00898_si_002.cif
_cod_data_source_block           2ClO42
_cod_database_code               4348030
_shelxl_version_number           2012-9
_shelx_estimated_absorpt_t_max   0.893
_shelx_estimated_absorpt_t_min   0.390
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N3) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(C39) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(C43) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(C9) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
3.a Aromatic/amide H refined with riding coordinates:
 C40(H40), C39(H39), C38(H38), C37(H37), C36(H36), C35(H35), C34(H34),
 C33(H33), C30(H30), C29(H29), C28(H28), C27(H27), C24(H24), C23(H23), C20(H20),
  C19(H19), C18(H18), C17(H17), C16(H16), C15(H15), C14(H14), C13(H13),
 C10(H10), C9(H9), C8(H8), C7(H7), C46(H46), C45(H45), C44(H44), C3(H3), C2(H2),
  C1(H1), C4(H4), C5(H5), C6(H6), C43(H43), C26(H26), C25(H25)
;
_shelx_res_checksum              49879
_shelx_hkl_checksum              19332
_olex2_submission_special_instructions 'No special instructions were received'