Multiple cluster CH activations and transformations of furan by triosmium carbonyl complexes.
Adams, Richard D.; Kiprotich, Emmanuel J.; Smith, Mark D.; Chemical communications (Cambridge, England) 54 (2018) 3464–3467; doi:10.1039/C8CC01532E

data_7121398
_publ_section_title
;
 Multiple cluster CH activations and transformations of furan by triosmium
 carbonyl complexes.
;
_journal_issue                   28
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              3464
_journal_page_last               3467
_journal_paper_doi               10.1039/C8CC01532E
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C22 H4 O19 Os6'
_chemical_formula_sum            'C22 H4 O19 Os6'
_chemical_formula_weight         1713.45
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2017-11-21
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2018-02-03 deposited with the CCDC.
2018-03-12 downloaded from the CCDC.
;
_cell_angle_alpha                82.9237(16)
_cell_angle_beta                 86.2639(16)
_cell_angle_gamma                67.6042(15)
_cell_formula_units_Z            2
_cell_length_a                   9.7044(5)
_cell_length_b                   11.2944(5)
_cell_length_c                   15.7359(7)
_cell_measurement_reflns_used    9802
_cell_measurement_temperature    100(2)
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_cell_measurement_theta_min      4.938
_cell_volume                     1582.19(13)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Bruker APEX3 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'PHOTON-100 CMOS 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 D8 QUEST diffractometer'
_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  0.0485
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            45497
_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         27.750
_diffrn_reflns_theta_min         2.237
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    24.077
_exptl_absorpt_correction_T_max  0.1515
_exptl_absorpt_correction_T_min  0.0615
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker, 2016'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.597
_exptl_crystal_description       block
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.337
_refine_diff_density_min         -2.051
_refine_diff_density_rms         0.289
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         7429
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0294
_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^)+(0.0078P)^2^+16.0471P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0467
_refine_ls_wR_factor_ref         0.0506
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6142
_reflns_number_total             7429
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc01532e2.cif
_cod_data_source_block           jk112017_0m_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7121393--7121398.cif.'
_cod_database_code               7121398
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.326
_shelx_estimated_absorpt_t_min   0.098
_olex2_refinement_description
;
1. Restrained distances
 H4-Os4
 1.8 with sigma of 0.02
 H4-Os5
 1.8 with sigma of 0.02
 H5-Os6
 1.8 with sigma of 0.02
 H5-Os4
 1.8 with sigma of 0.02
 H2-Os2
 1.8 with sigma of 0.02
 H2-Os3
 1.8 with sigma of 0.02
 H1-Os1
 1.8 with sigma of 0.02
 H1-Os2
 1.8 with sigma of 0.02
2.a Everything fixed:
 H2, H1
;
_olex2_submission_special_instructions 'No special instructions were received'