Reactions of Manganese and Rhenium Vinylidene Complexes with Hydrophosphoryl Compounds
Utegenov, Kamil I.; Krivykh, Vasilii V.; Mazhuga, Andrei M.; Chudin, Oleg S.; Smol'yakov, Aleksander F.; Dolgushin, Fedor M.; Goryunov, Evgenii I.; Ustynyuk, Nikolai A.; Organometallics 35 (2016) 3903–3913; doi:10.1021/acs.organomet.6b00626

data_4086809
_publ_section_title
;
 Reactions of Manganese and Rhenium Vinylidene Complexes with
 Hydrophosphoryl Compounds
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              3903
_journal_page_last               3913
_journal_paper_doi               10.1021/acs.organomet.6b00626
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C27 H12 F10 O3 P Re, C3 H6 O'
_chemical_formula_sum            'C30 H18 F10 O4 P Re'
_chemical_formula_weight         849.61
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                61.4248(8)
_cell_angle_beta                 73.9864(9)
_cell_angle_gamma                77.9876(9)
_cell_formula_units_Z            2
_cell_length_a                   10.6325(6)
_cell_length_b                   12.3889(7)
_cell_length_c                   12.8280(8)
_cell_measurement_reflns_used    9816
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      33.36
_cell_measurement_theta_min      2.38
_cell_volume                     1420.54(14)
_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      120(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  0.0190
_diffrn_reflns_av_unetI/netI     0.0189
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24369
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.999
_diffrn_reflns_theta_min         1.847
_exptl_absorpt_coefficient_mu    4.437
_exptl_absorpt_correction_T_max  0.665
_exptl_absorpt_correction_T_min  0.403
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.986
_exptl_crystal_description       prism
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.642
_refine_diff_density_min         -0.614
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         8278
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0147
_refine_ls_R_factor_gt           0.0138
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0104P)^2^+0.8002P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0325
_refine_ls_wR_factor_ref         0.0328
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8040
_reflns_number_total             8278
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00626_si_002.cif
_cod_data_source_block           repo
_cod_database_code               4086809
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.392
_shelx_estimated_absorpt_t_max   0.665
_shelx_res_checksum              72728
_shelx_hkl_checksum              5263