Reactivity of Cyclopentadienyl Molybdenum Compounds towards Formic Acid: Structural Characterization of CpMo(PMe3)(CO)2H, CpMo(PMe3)2(CO)H, [CpMo(μ-O)(μ-O2CH)]2, and [Cp*Mo(μ-O)(μ-O2CH)]2.
Neary, Michelle C.; Parkin, Gerard; Inorganic chemistry 56 (2017) 1511–1523; doi:10.1021/acs.inorgchem.6b02606

data_4345483
_publ_section_title
;
 Reactivity of Cyclopentadienyl Molybdenum Compounds towards Formic Acid:
 Structural Characterization of CpMo(PMe3)(CO)2H, CpMo(PMe3)2(CO)H,
 [CpMo(\m-O)(\m-O2CH)]2, and [Cp*Mo(\m-O)(\m-O2CH)]2.
;
_journal_issue                   3
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1511
_journal_page_last               1523
_journal_paper_doi               10.1021/acs.inorgchem.6b02606
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         'C12 H12 Mo2 O6'
_chemical_formula_sum            'C12 H12 Mo2 O6'
_chemical_formula_weight         444.10
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_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
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_cell_angle_gamma                90
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_cell_length_c                   12.999(7)
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_cell_measurement_theta_min      2.54
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_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
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_diffrn_reflns_av_R_equivalents  0.0697
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_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
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_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         32.327
_diffrn_reflns_theta_min         2.536
_exptl_absorpt_coefficient_mu    1.991
_exptl_absorpt_correction_T_max  0.746410
_exptl_absorpt_correction_T_min  0.472450
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   twinabs-2008/2
_exptl_crystal_colour            blue-red
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_refine_diff_density_max         1.580
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_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     91
_refine_ls_number_reflns         2243
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0347
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0363P)^2^+12.4396P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0827
_refine_ls_wR_factor_ref         0.0860
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_reflns_number_gt                1897
_reflns_number_total             2243
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            moformateta4_b.cif
_cod_data_source_block           moformateta4_b
_cod_original_cell_volume        1274.1(11)
_cod_database_code               4345483
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.596
_shelx_estimated_absorpt_t_max   0.925
_shelx_res_checksum              22247
_shelx_hkl_checksum              95954