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_4346764
_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_absolute_configuration unk
_chemical_formula_moiety         'C22 H16 Cl4 Mn N3 O3, F6 P'
_chemical_formula_sum            'C22 H16 Cl4 F6 Mn N3 O3 P'
_chemical_formula_weight         712.09
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2015-06-18
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 100.460(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.0245(6)
_cell_length_b                   14.7573(11)
_cell_length_c                   11.9344(9)
_cell_measurement_reflns_used    9092
_cell_measurement_temperature    105
_cell_measurement_theta_max      60.639
_cell_measurement_theta_min      2.606
_cell_volume                     1389.79(18)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection
;
APEX 2 (2013) Bruker AXS Inc., Madison, WI 53719-1173.
;
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      105
_diffrn_detector                 'CMOS Area detector'
_diffrn_detector_area_resol_mean 10.24
_diffrn_detector_type            'Bruker Photon 100 CMOS Detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       'k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker Venture Metaljet'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_collimation    'Focusing mirrors'
_diffrn_radiation_monochromator  'Helios MX Mirror Optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0533
_diffrn_reflns_av_unetI/netI     0.0406
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.987
_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            36892
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         60.745
_diffrn_reflns_theta_min         3.276
_diffrn_source                   'Metal Jet'
_diffrn_source_target            Ga
_diffrn_source_type              'Gallium Liquid Metal Jet Source'
_exptl_absorpt_coefficient_mu    5.634
_exptl_absorpt_correction_T_max  0.7519
_exptl_absorpt_correction_T_min  0.4160
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1686 before and 0.1125 after correction.
The Ratio of minimum to maximum transmission is 0.5533.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            Colorless
_exptl_crystal_colour_primary    Colorless
_exptl_crystal_density_diffrn    1.702
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             710
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.706
_refine_diff_density_min         -0.658
_refine_diff_density_rms         0.125
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.204(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     384
_refine_ls_number_reflns         5933
_refine_ls_number_restraints     82
_refine_ls_restrained_S_all      1.265
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0432
_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^)+(0.0823P)^2^+0.8235P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1182
_refine_ls_wR_factor_ref         0.1188
_reflns_Friedel_coverage         0.926
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                5815
_reflns_number_total             5933
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02087_si_008.cif
_cod_data_source_block           arst39
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' 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_cell_volume        1389.78(18)
_cod_database_code               4346764
_shelx_estimated_absorpt_t_max   0.806
_shelx_estimated_absorpt_t_min   0.399
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H1A(0.035) H1B(0.035) H1C(0.035) H3(0.024) H5A(0.04) H5B(0.04)
 H5C(0.04) H6A(0.048) H6B(0.048) H6C(0.048) H10(0.03) H11(0.034) H12(0.032)
 H16(0.033) H17(0.038) H18(0.038)
 Fixed X: H1A(1.1325) H1B(1.0417) H1C(1.1003) H3(0.8733) H5A(0.7799)
 H5B(0.7807) H5C(0.944) H6A(0.7232) H6B(0.6135) H6C(0.5212) H10(0.8794)
 H11(1.0523) H12(1.1219) H16(0.645) H17(0.3886) H18(0.2589)
 Fixed Y: H1A(0.4141) H1B(0.3242) H1C(0.4011) H3(0.3896) H5A(0.5964)
 H5B(0.491) H5C(0.536) H6A(0.2414) H6B(0.2835) H6C(0.2468) H10(0.3486)
 H11(0.4673) H12(0.5863) H16(0.8642) H17(0.8572) H18(0.7177)
 Fixed Z: H1A(0.3908) H1B(0.4249) H1C(0.5183) H3(0.2395) H5A(0.0934)
 H5B(0.062) H5C(0.1386) H6A(0.2621) H6B(0.1486) H6C(0.2478) H10(0.8216)
 H11(0.9067) H12(0.7959) H16(0.2004) H17(0.0738) H18(0.0234)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'