Synthesis and NMR Studies of [(C5Me5)Os(L)H2(H2)+] Complexes. Evidence of the Adoption of Different Structures by a Dihydrogen Complex in Solution and the Solid State
Gross, Christopher L.; Girolami, Gregory S.; Organometallics 26 (2007) 1658–; doi:10.1021/om061017e

data_4072771
_publ_section_title
;
 Synthesis and NMR Studies of [(C5Me5)Os(L)H2(H2)+] Complexes. Evidence of
 the Adoption of Different Structures by a Dihydrogen Complex in Solution
 and the Solid State
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1658
_journal_paper_doi               10.1021/om061017e
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C28 H52 B F4 Os P'
_chemical_formula_weight         696.68
_chemical_name_common            '[Cp*Os(PCy3)H4][BF4]'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                94.1140(10)
_cell_angle_beta                 90.0340(10)
_cell_angle_gamma                101.3690(10)
_cell_formula_units_Z            2
_cell_length_a                   8.9295(2)
_cell_length_b                   9.71790(10)
_cell_length_c                   17.18190(10)
_cell_measurement_temperature    199(2)
_cell_volume                     1457.79(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      199(2)
_diffrn_measured_fraction_theta_full 0.917
_diffrn_measured_fraction_theta_max 0.917
_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  0.0325
_diffrn_reflns_av_sigmaI/netI    0.0432
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            9506
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    4.469
_exptl_absorpt_correction_T_max  0.844
_exptl_absorpt_correction_T_min  0.529
_exptl_absorpt_correction_type   integration
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.434
_refine_diff_density_min         -1.408
_refine_diff_density_rms         0.140
_refine_ls_extinction_coef       0.0025(2)
_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_ref   1.081
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         6629
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0330
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+7.0947P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0702
_refine_ls_wR_factor_ref         0.0752
_reflns_number_gt                5953
_reflns_number_total             6629
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om061017esi20061105_085320.cif
_cod_data_source_block           osface
_cod_depositor_comments
;
 Removing duplicate rows from the ATOM_TYPE loop.

 Antanas Vaitkus,
 2018-08-10

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Integration'
changed to 'integration' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4072771