Nitrite reduction by a pyridinediimine complex with a proton-responsive secondary coordination sphere.
Kwon, Yubin M.; Delgado, Mayra; Zakharov, Lev N.; Seda, Takele; Gilbertson, John D.; Chemical communications (Cambridge, England) 52 (2016) 11016–11019; doi:10.1039/c6cc05962g

data_7124975
_publ_section_title
;
 Nitrite reduction by a pyridinediimine complex with a proton-responsive
 secondary coordination sphere.
;
_journal_issue                   73
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              11016
_journal_page_last               11019
_journal_paper_doi               10.1039/c6cc05962g
_journal_volume                  52
_journal_year                    2016
_chemical_formula_sum            'C29.5 H41 Cl Fe N4 O2'
_chemical_formula_weight         574.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-07-19 deposited with the CCDC.
2016-08-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.164(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.6385(9)
_cell_length_b                   13.7609(13)
_cell_length_c                   23.410(2)
_cell_measurement_reflns_used    6346
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.69
_cell_measurement_theta_min      2.29
_cell_volume                     3102.8(5)
_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-2013 (Sheldrick 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_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  0.0573
_diffrn_reflns_av_unetI/netI     0.0552
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            35837
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.995
_diffrn_reflns_theta_min         2.114
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.603
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.7059
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_description       block
_exptl_crystal_F_000             1220
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.110
_platon_squeeze_details
; 
The solvent molecule CH2Cl2 higly disordered around an 
inversion centers was treated be SQUEEZE. The correction 
of the X-ray data 90 electron/cell; the required value is 
84 electron/cell for two solvent molecules in the full unit cell.
;
_refine_diff_density_max         0.469
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         7488
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0437
_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^)+(0.0521P)^2^+0.1711P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1051
_refine_ls_wR_factor_ref         0.1119
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5426
_reflns_number_total             7488
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc05962g2.cif
_cod_data_source_block           mo_gilb160_0m
_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/RSC/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        3102.7(5)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C29.50 H41 Cl Fe N4 O2'
_cod_database_code               7124975
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.830
_shelx_estimated_absorpt_t_max   0.937
_shelx_res_checksum              3309