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_4348029
_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         'C43 H35 N10 O Os2, 3(Cl O4)'
_chemical_formula_sum            'C43 H35 Cl3 N10 O13 Os2'
_chemical_formula_weight         1386.56
_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'
_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                90
_cell_angle_beta                 116.892(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.693(3)
_cell_length_b                   23.662(3)
_cell_length_c                   20.977(3)
_cell_measurement_reflns_used    5012
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.12
_cell_measurement_theta_min      3.10
_cell_volume                     9160(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 0.969
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0843
_diffrn_reflns_av_unetI/netI     0.0651
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            74261
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         3.031
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    5.796
_exptl_absorpt_correction_T_max  0.4215
_exptl_absorpt_correction_T_min  0.4215
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.011
_exptl_crystal_density_meas      plate
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             5360
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.13
_refine_diff_density_max         2.816
_refine_diff_density_min         -1.452
_refine_diff_density_rms         0.199
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1279
_refine_ls_number_reflns         16059
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0379
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0281P)^2^+20.7536P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0895
_refine_ls_wR_factor_ref         0.0989
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13697
_reflns_number_total             16059
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00898_si_001.cif
_cod_data_source_block           1ClO43
_cod_database_code               4348029
_shelxl_version_number           2012-9
_shelx_estimated_absorpt_t_max   0.520
_shelx_estimated_absorpt_t_min   0.236
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C47(H47), C24(H24), C4(H4), C66(H66), C23(H23), C57(H57), C67(H67), C3(H3),
 C1(H1), C83(H83), C86(H86), C56(H56), C27(H27), C43(H43), C14(H14), C44(H44),
 C2(H2), C34(H34), C46(H46), C48(H48), C17(H17), C76(H76), C22(H22), C79(H79),
 C63(H63), C33(H33), C7(H7), C49(H49), C75(H75), C65(H65), C20(H20), C15(H15),
 C13(H13), C70(H70), C10(H10), C73(H73), C45(H45), C42(H42), C50(H50), C12(H12),
  C64(H64), C11(H11), C80(H80), C78(H78), C58(H58), C68(H68), C16(H16),
 C41(H41), C25(H25), C21(H21), C53(H53), C35(H35), C55(H55), C74(H74), C40(H40),
  C77(H77), C85(H85), C84(H84), C26(H26), C6(H6), C5(H5), C69(H69), C60(H60),
 C32(H32), C30(H30), C37(H37), C59(H59), C36(H36), C54(H54), C31(H31)
;
_shelx_res_checksum              35986
_shelx_hkl_checksum              8580
_olex2_submission_special_instructions 'No special instructions were received'