Flexibility and lability of a phenyl ligand in hetero-organometallic 3d metal-Sn(IV) compounds and their catalytic activity in Baeyer‒Villiger oxidation of cyclohexanone
Hazra, Susanta; Martins, Nuno M. R.; Kuznetsov, Maxim L.; Guedes da Silva, M. Fátima C.; Pombeiro, Armando J. L.; Dalton Trans.  (2017) –; doi:10.1039/C7DT02534C

data_7043916
_publ_section_title
;
 Flexibility and lability of a phenyl ligand in hetero-organometallic 3d
 metal-Sn(IV) compounds and their catalytic activity in Baeyer--Villiger
 oxidation of cyclohexanone
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02534C
_journal_year                    2017
_chemical_formula_sum            'C22 H21 Co N2 O3'
_chemical_formula_weight         420.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-03-25 deposited with the CCDC.
2017-08-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.1230(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.206(2)
_cell_length_b                   14.7370(17)
_cell_length_c                   6.7877(8)
_cell_measurement_reflns_used    3341
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      22.33
_cell_measurement_theta_min      2.76
_cell_volume                     1821.1(4)
_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 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0844
_diffrn_reflns_av_unetI/netI     0.0585
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            18159
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.103
_diffrn_reflns_theta_max         25.103
_diffrn_reflns_theta_min         2.237
_exptl_absorpt_coefficient_mu    0.969
_exptl_absorpt_correction_T_max  0.899
_exptl_absorpt_correction_T_min  0.861
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_description       Plate
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.464
_refine_diff_density_min         -0.379
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.01(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     279
_refine_ls_number_reflns         3208
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0707
_refine_ls_R_factor_gt           0.0471
_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^)+(0.0324P)^2^+2.0311P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0846
_refine_ls_wR_factor_ref         0.0920
_reflns_Friedel_coverage         0.995
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                2616
_reflns_number_total             3208
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02534c2.cif
_cod_data_source_block           1A-Co
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        1821.2(4)
_cod_database_code               7043916
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.876
_shelx_estimated_absorpt_t_max   0.926
_shelx_res_checksum              78487