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_4345482
_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         'C22 H32 Mo2 O6'
_chemical_formula_sum            'C22 H32 Mo2 O6'
_chemical_formula_weight         584.35
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.055(9)
_cell_length_b                   20.208(13)
_cell_length_c                   7.933(5)
_cell_measurement_reflns_used    5228
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      27.80
_cell_measurement_theta_min      2.76
_cell_volume                     2253(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0910
_diffrn_reflns_av_unetI/netI     0.0666
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            13020
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.016
_exptl_absorpt_coefficient_mu    1.148
_exptl_absorpt_correction_T_max  .7456
_exptl_absorpt_correction_T_min  .4707
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            blue-orange
_exptl_crystal_density_diffrn    1.723
_exptl_crystal_description       plate
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.799
_refine_diff_density_min         -1.637
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.206
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         2376
_refine_ls_number_restraints     85
_refine_ls_restrained_S_all      1.190
_refine_ls_R_factor_all          0.0855
_refine_ls_R_factor_gt           0.0580
_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^)+(0.0134P)^2^+16.7753P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1267
_refine_ls_wR_factor_ref         0.1372
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1717
_reflns_number_total             2376
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cpstarformated_b.cif
_cod_data_source_block           cpstarformated_b
_cod_original_cell_volume        2253(3)
_cod_database_code               4345482
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.856
_shelx_estimated_absorpt_t_max   0.977
_shelx_res_checksum              89960
_shelx_hkl_checksum              839