A mononuclear nonheme {FeNO}<sup>6</sup> complex: synthesis and structural and spectroscopic characterization.
Hong, Seungwoo; Yan, James J.; Karmalkar, Deepika G.; Sutherlin, Kyle D.; Kim, Jin; Lee, Yong-Min; Goo, Yire; Mascharak, Pradip K.; Hedman, Britt; Hodgson, Keith O.; Karlin, Kenneth D.; Solomon, Edward I.; Nam, Wonwoo; Chemical science 9 (2018) 6952–6960; doi:10.1039/c8sc01962b

data_1549707
_publ_section_title
;
 A mononuclear nonheme {FeNO}<sup>6</sup> complex: synthesis and
 structural and spectroscopic characterization.
;
_journal_issue                   34
_journal_name_full               'Chemical science'
_journal_page_first              6952
_journal_page_last               6960
_journal_paper_doi               10.1039/c8sc01962b
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety         'C19 H22 Fe N5 O5, C24 H20 P, C4 H10 O'
_chemical_formula_sum            'C47 H52 Fe N5 O6 P'
_chemical_formula_weight         869.75
_chemical_name_common            Fe(IV)-nitroxyl
_chemical_name_systematic        '[Fe(NO)(TAML)]-'
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2017-09-14 deposited with the CCDC.
2018-07-19 downloaded from the CCDC.
;
_cell_angle_alpha                93.792(3)
_cell_angle_beta                 92.468(3)
_cell_angle_gamma                90.347(3)
_cell_formula_units_Z            2
_cell_length_a                   12.7848(8)
_cell_length_b                   13.0223(8)
_cell_length_c                   13.1304(9)
_cell_measurement_reflns_used    72796
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.441
_cell_measurement_theta_min      2.134
_cell_volume                     2179.2(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0233
_diffrn_reflns_av_unetI/netI     0.0155
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            72796
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.441
_diffrn_reflns_theta_min         2.134
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.437
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             916
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.130
_exptl_transmission_factor_max   0.746
_exptl_transmission_factor_min   0.680
_refine_diff_density_max         1.554
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     549
_refine_ls_number_reflns         10889
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0348
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0412P)^2^+1.8412P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0874
_refine_ls_wR_factor_ref         0.0938
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9570
_reflns_number_total             10889
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc01962b2.cif
_cod_data_source_block           KJ028-1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 1549707--1549708.cif.
;
_cod_database_code               1549707
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.873
_shelx_estimated_absorpt_t_max   0.945
_shelx_res_checksum              41693