Single-Crystal 31P NMR and X-ray Diffraction Study of a Molybdenum Phosphine Complex: (5-Methyldibenzophosphole)pentacarbonylmolybdenum(0)
Klaus Eichele; Roderick E. Wasylishen; Kalyani Maitra; John H. Nelson; James F. Britten; Inorganic Chemistry 36 (1997) 3539–3544; doi:10.1021/ic970260q

data_4323513
_publ_section_title
;
 Single-Crystal 31P NMR and X-ray Diffraction Study of a Molybdenum
 Phosphine Complex: (5-Methyldibenzophosphole)pentacarbonylmolybdenum(0)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3539
_journal_page_last               3544
_journal_paper_doi               10.1021/ic970260q
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C18 H11 Mo O5 P'
_chemical_formula_weight         434.18
_chemical_name_systematic        ?
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 122.135(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   31.113(2)
_cell_length_b                   7.7917(5)
_cell_length_c                   17.9522(12)
_cell_measurement_reflns_used    27
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      12.49
_cell_measurement_theta_min      5.11
_cell_volume                     3685.3(4)
_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-93 (Sheldrick, 1993)'
_diffrn_ambient_temperature      298(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  0.0161
_diffrn_reflns_av_sigmaI/netI    0.0185
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            3022
_diffrn_reflns_theta_max         22.49
_diffrn_reflns_theta_min         2.27
_diffrn_standards_decay_%        0.69
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.822
_exptl_absorpt_correction_T_max  0.6118
_exptl_absorpt_correction_T_min  0.5626
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            pale_yellow
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_description       rhomb
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          .40
_exptl_crystal_size_mid          .55
_exptl_crystal_size_min          .68
_refine_diff_density_max         0.279
_refine_diff_density_min         -0.223
_refine_diff_density_rms         0.046
_refine_ls_extinction_coef       0.00099(9)
_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   1.104
_refine_ls_goodness_of_fit_obs   1.131
_refine_ls_hydrogen_treatment    'riding model with fixed U'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         2407
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_restrained_S_obs      1.131
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_obs          0.0245
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0281P)^2^+4.3206P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0609
_refine_ls_wR_factor_obs         0.0584
_reflns_number_observed          2137
_reflns_number_total             2407
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic970260q.cif
_cod_data_source_block           vjc129
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0281P)^2^+4.3206P] 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^)+(0.0281P)^2^+4.3206P] 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        3685.2(4)
_cod_database_code               4323513