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_7124974
_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 H41 F6 Fe N4 O2 P'
_chemical_formula_weight         678.48
_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   mixed
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2016-07-19 deposited with the CCDC.
2016-08-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.237(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.0286(15)
_cell_length_b                   8.7204(7)
_cell_length_c                   17.6555(12)
_cell_measurement_reflns_used    3136
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      65.67
_cell_measurement_theta_min      4.26
_cell_volume                     3195.6(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-2013 (Sheldrick 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1332
_diffrn_reflns_av_unetI/netI     0.0980
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            27682
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         66.754
_diffrn_reflns_theta_min         2.128
_diffrn_source                   'micro-focus Incoatec I\mS'
_exptl_absorpt_coefficient_mu    4.857
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.5846
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_description       plate
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.014
_exptl_crystal_size_mid          0.012
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.501
_refine_diff_density_min         -0.654
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         5641
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.1132
_refine_ls_R_factor_gt           0.0647
_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^)+(0.0730P)^2^+1.5350P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1394
_refine_ls_wR_factor_ref         0.1614
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3555
_reflns_number_total             5641
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc05962g2.cif
_cod_data_source_block           gilb174a
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7124974
_shelx_estimated_absorpt_t_min   0.935
_shelx_estimated_absorpt_t_max   0.953
_shelxl_version_number           2013-4
_shelx_res_checksum              85193