Octadecacarbonylhexaosmium chloroform solvate
Blake, Alexander J.; Johnson, Brian F.G.; Nairn, Jacqueline G.M.; Acta Crystallographica Section C 50 (1994) 1052–1054; doi:10.1107/S0108270194000363

data_2009870
_publ_section_title
;
 Octadecacarbonylhexaosmium chloroform solvate
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1052
_journal_page_last               1054
_journal_paper_doi               10.1107/S0108270194000363
_journal_volume                  50
_journal_year                    1994
_chemical_formula_moiety         'C18 O18 Os6 , C H Cl3'
_chemical_formula_structural     Os6(CO)18.CHCl3
_chemical_formula_sum            'C19 H Cl3 O18 Os6'
_chemical_formula_weight         1764.75
_chemical_name_systematic
;
Hexaosmium octadecarbonyl-chloroform solvate(1:1)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 91.47(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.074(3)
_cell_length_b                   27.293(9)
_cell_length_c                   11.286(3)
_cell_measurement_reflns_used    32
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      16
_cell_measurement_theta_min      15
_cell_volume                     3102.1(16)
_computing_cell_refinement       'Stoe DIF4'
_computing_data_collection       'Stoe DIF4'
_computing_data_reduction        'Stoe REDU4'
_computing_molecular_graphics    SHELXTL/PC
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150.0(2)
_diffrn_measurement_device       'Stoe Stadi-4 four-circle diffractometer'
_diffrn_measurement_method       '\w scans with on-line profile fitting'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_sigmaI/netI    0.0323
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4274
_diffrn_reflns_theta_max         22.55
_diffrn_reflns_theta_min         2.51
_diffrn_standards_decay_%        <2
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    24.814
_exptl_absorpt_correction_T_max  0.117
_exptl_absorpt_correction_T_min  0.048
_exptl_absorpt_correction_type   'Semi-empirical (SHELXTL/PC)'
_exptl_crystal_colour            'Dark red'
_exptl_crystal_density_diffrn    3.779
_exptl_crystal_description       Block
_exptl_crystal_F_000             3064
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.717
_refine_diff_density_min         -1.405
_refine_ls_extinction_coef       0.00010(2)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.036
_refine_ls_goodness_of_fit_obs   1.038
_refine_ls_hydrogen_treatment    'H atoms in a fixed, calculated position'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         3851
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_restrained_S_obs      1.038
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_obs          0.0356
_refine_ls_shift/esd_max         -0.171
_refine_ls_shift/esd_mean        0.026
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;calc w = 1/[\s^2^(F~o~^2^)+(0.0439P)^2^+157.2638P]
where P = (F~o~^2^+2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.0970
_refine_ls_wR_factor_obs         0.0872
_reflns_number_observed          3335
_reflns_number_total             3855
_reflns_observed_criterion       >2\s(I)
_cod_data_source_file            ha1094.cif
_cod_data_source_block           os3dec
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2009870