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_4086810
_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 H22 O2 P Re S'
_chemical_formula_sum            'C27 H22 O2 P Re S'
_chemical_formula_weight         627.67
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 96.509(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.8861(6)
_cell_length_b                   18.3729(14)
_cell_length_c                   18.2690(16)
_cell_measurement_reflns_used    9456
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.6
_cell_measurement_theta_min      2.2
_cell_volume                     2296.5(3)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0292
_diffrn_reflns_av_unetI/netI     0.0195
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            31531
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.997
_diffrn_reflns_theta_min         2.244
_exptl_absorpt_coefficient_mu    5.475
_exptl_absorpt_correction_T_max  0.611
_exptl_absorpt_correction_T_min  0.277
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.815
_exptl_crystal_description       prism
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         2.301
_refine_diff_density_min         -1.418
_refine_diff_density_rms         0.111
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         5524
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0235
_refine_ls_R_factor_gt           0.0224
_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^)+(0.0162P)^2^+5.9683P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0509
_refine_ls_wR_factor_ref         0.0514
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5332
_reflns_number_total             5524
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00626_si_002.cif
_cod_data_source_block           repsinv
_cod_database_code               4086810
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.290
_shelx_estimated_absorpt_t_max   0.611
_shelx_res_checksum              72972
_shelx_hkl_checksum              11403