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_4072770
_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 H34 B F4 Os P'
_chemical_formula_weight         678.53
_chemical_name_common            '[Cp*Os(PPh3)H4][BF4]'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 99.0620(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.5516(4)
_cell_length_b                   27.6809(10)
_cell_length_c                   9.4129(4)
_cell_measurement_temperature    198(2)
_cell_volume                     2714.98(18)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      198(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  0.0409
_diffrn_reflns_av_sigmaI/netI    0.0405
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            17483
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    4.798
_exptl_absorpt_correction_T_max  0.989
_exptl_absorpt_correction_T_min  0.607
_exptl_absorpt_correction_type   gaussian
_exptl_crystal_density_diffrn    1.660
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.287
_refine_diff_density_min         -1.268
_refine_diff_density_rms         0.138
_refine_ls_extinction_coef       0.00099(10)
_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   1.127
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         6463
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.131
_refine_ls_restrained_S_obs      1.105
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0166P)^2^+13.0618P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0863
_refine_ls_wR_factor_ref         0.0746
_reflns_number_gt                5135
_reflns_number_total             6468
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om061017esi20061105_085304.cif
_cod_data_source_block           osh4abs
_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 'Monoclinic' changed to 'monoclinic'
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 'Gaussian'
changed to 'gaussian' 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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0166P)^2^+13.0618P] 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^)+(0.0166P)^2^+13.0618P] 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        2715.0(2)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4072770