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_4116914
_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 H70 K N O6 Os P2'
_chemical_formula_weight         844.12
_chemical_name_systematic
; 
 ? 
;
_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'
_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                 104.608(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.595(3)
_cell_length_b                   21.667(4)
_cell_length_c                   16.676(3)
_cell_measurement_temperature    173(2)
_cell_volume                     4054.1(15)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_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  0.0315
_diffrn_reflns_av_sigmaI/netI    0.0585
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12159
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.52
_exptl_absorpt_coefficient_mu    3.363
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_F_000             1744
_refine_diff_density_max         0.835
_refine_diff_density_min         -1.317
_refine_diff_density_rms         0.116
_refine_ls_extinction_coef       0.00045(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.951
_refine_ls_goodness_of_fit_obs   1.064
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         11661
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.953
_refine_ls_restrained_S_obs      1.064
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_obs          0.0323
_refine_ls_shift/esd_max         0.013
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0305P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0756
_refine_ls_wR_factor_obs         0.0724
_reflns_number_observed          8646
_reflns_number_total             11662
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja9817693_2.cif
_cod_data_source_block           s9731
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0305P)^2^+0.0000P] 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^)+(0.0305P)^2^+0.0000P] 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        4054.2(14)
_cod_original_formula_sum        'C31 H4 H66 K N O6 Os P2'
_cod_database_code               4116914