New Polyhydride Anions and Proton-Hydride Hydrogen Bonding in Their Ion Pairs. X-ray Crystal Structure Determinations of Q[mer-Os(H)3(CO)(PiPr3)2], Q = [K(18-crown-6)] and Q = [K(1-aza-18-crown-6)]
Dmitry G. Gusev; Alan J. Lough; Robert H. Morris; Journal of the American Chemical Society 120 (1998) 13138–13147; doi:10.1021/ja9817693

data_4116913
_publ_section_title
;
 New Polyhydride Anions and Proton-Hydride Hydrogen Bonding in Their Ion
 Pairs. X-ray Crystal Structure Determinations of
 Q[mer-Os(H)3(CO)(PiPr3)2], Q = [K(18-crown-6)] and Q =
 [K(1-aza-18-crown-6)]
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13138
_journal_page_last               13147
_journal_paper_doi               10.1021/ja9817693
_journal_volume                  120
_journal_year                    1998
_chemical_formula_sum            'C31 H69 K O7 Os P2'
_chemical_formula_weight         845.10
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 92.542(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   47.790(7)
_cell_length_b                   11.517(2)
_cell_length_c                   21.428(4)
_cell_measurement_reflns_used    44
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      12.00
_cell_measurement_theta_min      4.81
_cell_volume                     11782(3)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0682
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -60
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            12838
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.04
_diffrn_standards_decay_%        7.43
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.473
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             5232
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         3.505
_refine_diff_density_min         -1.841
_refine_diff_density_rms         0.164
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.37(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.035
_refine_ls_goodness_of_fit_obs   1.066
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1145
_refine_ls_number_reflns         12837
_refine_ls_number_restraints     578
_refine_ls_restrained_S_all      1.013
_refine_ls_restrained_S_obs      1.037
_refine_ls_R_factor_all          0.0803
_refine_ls_R_factor_obs          0.0590
_refine_ls_shift/esd_max         -0.018
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0508P)^2^+176.6696P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1367
_refine_ls_wR_factor_obs         0.1254
_reflns_number_observed          10394
_reflns_number_total             12838
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja9817693_1.cif
_cod_data_source_block           s9746
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0508P)^2^+176.6696P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0508P)^2^+176.6696P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        11781.7(31)
_cod_database_code               4116913