Crystal structure of aqua-azido-κ1 N-(6,6′-((propane-1,3-diylbis(azanylylidene))bis(methanylylidene))bis(3-bromophenolato)-κ4 N,N′,O,O′iron(III), C17H16Br2FeN5O3
Xiao, Jianchang; Zhou, Cun; Huang, Meifen; Tan, Hui; Wu, Qiong; Zeitschrift für Kristallographie - New Crystal Structures 235 (2020) 903–904; doi:10.1515/ncrs-2020-0091

data_8105325
_publ_section_title
;
 Crystal structure of aqua-azido-\k1
 N-(6,6&#x2032;-((propane-1,3-diylbis(azanylylidene))bis(methanylylidene))bis(3-bromophenolato)-\k4
 N,N&#x2032;,O,O&#x2032;iron(III), C17H16Br2FeN5O3
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              903
_journal_page_last               904
_journal_paper_doi               10.1515/ncrs-2020-0091
_journal_volume                  235
_journal_year                    2020
_chemical_formula_moiety         'C17 H16 Br2 Fe N5 O3'
_chemical_formula_sum            'C17 H16 Br2 Fe N5 O3'
_chemical_formula_weight         554.02
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.9307(9)
_cell_length_b                   14.8166(17)
_cell_length_c                   22.923(2)
_cell_measurement_reflns_used    7213
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      62.716
_cell_measurement_theta_min      3.857
_cell_volume                     4052.2(7)
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.862
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0641
_diffrn_reflns_av_unetI/netI     0.0637
_diffrn_reflns_Laue_measured_fraction_full 0.862
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            7213
_diffrn_reflns_point_group_measured_fraction_full 0.862
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         62.716
_diffrn_reflns_theta_min         3.857
_exptl_absorpt_coefficient_mu    10.842
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.33849
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            'clear reddish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.816
_exptl_crystal_description       block
_exptl_crystal_F_000             2184
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.841
_refine_diff_density_min         -0.851
_refine_diff_density_rms         0.148
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         3157
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.0982
_refine_ls_R_factor_gt           0.0750
_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^)+(0.1419P)^2^+3.2933P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2139
_refine_ls_wR_factor_ref         0.2497
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2284
_reflns_number_total             3157
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2020-0091_suppl.cif
_cod_data_source_block           e19
_cod_database_code               8105325
_shelx_estimated_absorpt_t_max   0.356
_shelx_estimated_absorpt_t_min   0.276
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C9-C10
 1.35 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C8) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(N2) \\sim
Ueq, Uanis(N3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
4.a Rotating group:
 O3(H3A,H3B)
4.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B)
4.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C7(H7), C11(H11), C13(H13), C14(H14), C16(H16)
;