Intramolecular C-C Bond Coupling of Nitriles to a Diimine Ligand in Group 7 Metal Tricarbonyl Complexes.
Yempally, Veeranna; Fan, Wai Yip; Arndtsen, Bruce A.; Bengali, Ashfaq A.; Inorganic chemistry 54 (2015) 11441–11449; doi:10.1021/acs.inorgchem.5b02087

data_4346759
_publ_section_title
;
 Intramolecular C-C Bond Coupling of Nitriles to a Diimine Ligand in Group
 7 Metal Tricarbonyl Complexes.
;
_journal_issue                   23
_journal_name_full               'Inorganic chemistry'
_journal_page_first              11441
_journal_page_last               11449
_journal_paper_doi               10.1021/acs.inorgchem.5b02087
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C22 H17 Cl4 F6 N3 O3 P Re'
_chemical_formula_sum            'C22 H17 Cl4 F6 N3 O3 P Re'
_chemical_formula_weight         844.35
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 100.12(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.9598(16)
_cell_length_b                   14.847(3)
_cell_length_c                   11.959(2)
_cell_measurement_reflns_used    4122
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.877
_cell_measurement_theta_min      2.208
_cell_volume                     1391.3(5)
_computing_cell_refinement
'SHELXTL, Acta Cryst., Sect. A 2008, 64, 112-122.'
_computing_data_collection       'APEX v2014.11.0'
_computing_data_reduction        'Saint, APEX v2014.11.0.'
_computing_molecular_graphics    Ortep3
_computing_publication_material  'APEX v2014.11.0.'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution
'SHELXT, Acta Cryst., Sect. A 2015, A71, 3-8.'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker AXS D8 Venture '
_diffrn_measurement_method       'profile data from \q/2\q scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0452
_diffrn_reflns_av_unetI/netI     0.0707
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17738
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.877
_diffrn_reflns_theta_min         2.208
_exptl_absorpt_coefficient_mu    4.881
_exptl_absorpt_correction_T_max  0.679
_exptl_absorpt_correction_T_min  0.233
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Sadabs
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    2.016
_exptl_crystal_description       'prism frag'
_exptl_crystal_F_000             812
_exptl_crystal_size_max          0.422
_exptl_crystal_size_mid          0.194
_exptl_crystal_size_min          0.086
_refine_diff_density_max         0.971
_refine_diff_density_min         -0.754
_refine_diff_density_rms         0.138
_refine_ls_abs_structure_details
;
 Flack x determined using 2526 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.028(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         6514
_refine_ls_number_restraints     286
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0324
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0092P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0635
_refine_ls_wR_factor_ref         0.0660
_reflns_Friedel_coverage         0.895
_reflns_Friedel_fraction_full    0.968
_reflns_Friedel_fraction_max     0.966
_reflns_number_gt                5807
_reflns_number_total             6514
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02087_si_004.cif
_cod_data_source_block           shelx
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4346759
_shelx_estimated_absorpt_t_min   0.233
_shelx_estimated_absorpt_t_max   0.679
_shelxl_version_number           2014/6
_shelx_res_checksum              13039
_shelx_hkl_checksum              70445