Formation of organometallic hydroxo and oxo complexes by oxidation of transition metal hydrides in the presence of water. X-Ray structures of [CpMo(OH)(PMe3)3][BF4] and [CpMo(O)(PMe3)2][BF4]
Fettinger, James C.; Kraatz, Heinz-Bernhard; Poli, Rinaldo; Quadrelli, E. Alessandra; Journal of the Chemical Society, Dalton Transactions  (1999) 497–; doi:10.1039/a807111j

data_7027115
_publ_section_title
;
 Formation of organometallic hydroxo and oxo complexes by oxidation of
 transition metal hydrides in the presence of water. X-Ray structures of
 [CpMo(OH)(PMe3)3][BF4] and [CpMo(O)(PMe3)2][BF4]
;
_journal_issue                   3
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              497
_journal_paper_doi               10.1039/a807111j
_journal_year                    1999
_chemical_formula_sum            'C11 H23 B F4 Mo O P2'
_chemical_formula_weight         415.98
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           40
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'A 2 -2a'
_symmetry_space_group_name_H-M   'A m a 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.289(16)
_cell_length_b                   15.201(2)
_cell_length_c                   6.6459(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13.7
_cell_measurement_theta_min      7.8
_cell_volume                     1746.6(16)
_computing_cell_refinement       'Enraf-Nonius CAD-4 control program'
_computing_data_collection       'Enraf-Nonius CAD-4 control program'
_computing_data_reduction        'Harms, XCAD4, 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      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       '\w:2\q 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  0.0336
_diffrn_reflns_av_sigmaI/netI    0.0873
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            969
_diffrn_reflns_theta_max         22.97
_diffrn_reflns_theta_min         2.36
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.963
_exptl_absorpt_correction_T_max  0.8101
_exptl_absorpt_correction_T_min  0.7352
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'reddish orange'
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_description       Plate
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.409
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.087
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.09(16)
_refine_ls_extinction_coef       0.0007(5)
_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   1.068
_refine_ls_goodness_of_fit_obs   1.128
_refine_ls_matrix_type           full
_refine_ls_number_parameters     141
_refine_ls_number_reflns         692
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.059
_refine_ls_restrained_S_obs      1.114
_refine_ls_R_factor_all          0.0782
_refine_ls_R_factor_obs          0.0391
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0289P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0801
_refine_ls_wR_factor_obs         0.0715
_reflns_number_observed          534
_reflns_number_total             692
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            807111jsup1.cif
_cod_data_source_block           UM079
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0289P)^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^)+(0.0289P)^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_sg_symbol_H-M      Ama2
_cod_database_code               7027115