Crystal structure of di-μ2-hydroxido-tetrakis(6-methylpyridine-2-carboxylato-k2 N,O) diiron(III) trihydrate C28H32Fe2N4O13
Cui, Hong-Meng; Zeitschrift für Kristallographie - New Crystal Structures 237 (2022) 793–795; doi:10.1515/ncrs-2022-0240

data_8107218
_publ_section_title
;
 Crystal structure of
 di-\m2-hydroxido-tetrakis(6-methylpyridine-2-carboxylato-k2 N,O)
 diiron(III) trihydrate C28H32Fe2N4O13
;
_journal_issue                   5
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              793
_journal_page_last               795
_journal_paper_doi               10.1515/ncrs-2022-0240
_journal_volume                  237
_journal_year                    2022
_chemical_formula_moiety         'C28 H26 Fe2 N4 O10, 3(H2 O)'
_chemical_formula_sum            'C28 H32 Fe2 N4 O13'
_chemical_formula_weight         744.27
_chemical_name_systematic
;
[di-\m-hydroxidotetrakis(6-methylpyridine-2-carboxylato)-di-iron(III)]-
hydrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_cell_angle_alpha                90
_cell_angle_beta                 95.190(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.0964(3)
_cell_length_b                   13.4889(5)
_cell_length_c                   14.0543(5)
_cell_measurement_reflns_used    5052
_cell_measurement_temperature    173
_cell_measurement_theta_max      28.7817
_cell_measurement_theta_min      2.7910
_cell_volume                     1528.60(10)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.886
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.886
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10287
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.886
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.878
_diffrn_reflns_theta_min         2.799
_exptl_absorpt_coefficient_mu    1.024
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_description       block
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.448
_refine_diff_density_min         -0.573
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3566
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0405
_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^)+(0.0537P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0908
_refine_ls_wR_factor_ref         0.0972
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2670
_reflns_number_total             3566
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2022-0240_suppl.cif
_cod_data_source_block           p
_cod_database_code               8107218
_shelx_estimated_absorpt_t_max   0.951
_shelx_estimated_absorpt_t_min   0.845
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H1W of O1W
 At 1.5 times of:
  All C(H,H,H) groups, H2WA of O2W
2.a Free rotating group:
 O1W(H1W), O2W(H2WA,H2WB)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5A), C10(H10), C11(H11), C12(H12)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              67898
_shelx_hkl_checksum              4906
_olex2_submission_special_instructions 'No special instructions were received'