Mixed valency in a neutral 1D Fe-chloranilate coordination polymer.
Clutterbuck, Katelyn M.; Abrahams, Brendan F.; Hudson, Timothy A.; van Koeverden, Martin P.; Dalton transactions (Cambridge, England : 2003) 51 (2022) 9199–9205; doi:10.1039/d1dt04368d

data_7710413
_publ_section_title
;
 Mixed valency in a neutral 1D Fe-chloranilate coordination polymer.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9199
_journal_page_last               9205
_journal_paper_doi               10.1039/d1dt04368d
_journal_volume                  51
_journal_year                    2022
_chemical_formula_moiety         'C26 H16 F2 N4 O4 Zn'
_chemical_formula_sum            'C26 H16 F2 N4 O4 Zn'
_chemical_formula_weight         551.80
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-04-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-12-29 deposited with the CCDC.	2022-06-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.072(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.3388(4)
_cell_length_b                   9.7015(2)
_cell_length_c                   13.8237(3)
_cell_measurement_reflns_used    5086
_cell_measurement_temperature    100
_cell_measurement_theta_max      77.2430
_cell_measurement_theta_min      5.2560
_cell_volume                     2174.54(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     51.00  77.00   0.50    0.52    --   47.57  51.00  91.00   52
  2  \w     94.00 124.00   0.50    2.00    --  107.75  51.00  91.00   60
  3  \w    137.00 171.00   0.50    2.00    --  107.75  51.00  91.00   68
  4  \w    137.00 176.00   0.50    2.00    --  107.75  30.00   0.00   78
  5  \w     97.00 130.00   0.50    2.00    --  107.75  30.00   0.00   66
  6  \w    147.00 173.00   0.50    2.00    --  107.75  45.00-150.00   52
  7  \w    103.00 144.00   0.50    2.00    --  107.75  45.00-150.00   82
  8  \w     40.00  67.00   0.50    2.00    --  107.75 -61.00 150.00   54
  9  \w     37.00  63.00   0.50    2.00    --  107.75 -61.00  90.00   52
 10  \w     40.00  69.00   0.50    2.00    --  107.75 -61.00  60.00   58
 11  \w     37.00  91.00   0.50    2.00    --  107.75 -77.00   0.00  108
 12  \w     35.00  91.00   0.50    2.00    --  107.75 -77.00 -90.00  112
 13  \w     40.00  69.00   0.50    2.00    --  107.75 -61.00-150.00   58
 14  \w    110.00 136.00   0.50    2.00    --  107.75 125.00 -60.00   52
 15  \w    145.00 170.00   0.50    2.00    --  107.75 125.00 -60.00   50
 16  \w     -7.00  27.00   0.50    0.52    --   47.57 -19.00 120.00   68
 17  \w    -19.00   7.00   0.50    0.52    --   47.57 -51.00 -54.00   52
 18  \w     15.00  42.00   0.50    0.52    --   47.57 -51.00 -54.00   54
 19  \w    -57.00  25.00   0.50    0.52    --  -47.57  51.00  91.00  164
 20  \w    -42.00 -16.00   0.50    2.00    --  -86.25  45.00  60.00   52
 21  \w    -42.00 -16.00   0.50    2.00    --  -86.25  51.00  91.00   52
 22  \w    -50.00 -17.00   0.50    2.00    --  -86.25  45.00  30.00   66
 23  \w    -50.00 -20.00   0.50    2.00    --  -86.25  45.00 -90.00   60
 24  \w    -37.00 -12.00   0.50    2.00    --  -86.25  30.00-120.00   50
 25  \w    -50.00 -15.00   0.50    2.00    --  -86.25  45.00-180.00   70
 26  \w   -156.00 -72.00   0.50    2.00    --  -86.25 -51.00 -54.00  168
 27  \w   -118.00 -35.00   0.50    0.52    --  -47.57 -51.00 -54.00  166
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0741485000
_diffrn_orient_matrix_UB_12      -0.0935448000
_diffrn_orient_matrix_UB_13      -0.0342277000
_diffrn_orient_matrix_UB_21      -0.0096218000
_diffrn_orient_matrix_UB_22      -0.0336796000
_diffrn_orient_matrix_UB_23      0.1068849000
_diffrn_orient_matrix_UB_31      -0.0586109000
_diffrn_orient_matrix_UB_32      0.1238711000
_diffrn_orient_matrix_UB_33      0.0033095000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0486
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7724
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.590
_diffrn_reflns_theta_min         5.313
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.123
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.783
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.685
_exptl_crystal_description       needle
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.131
_exptl_crystal_size_mid          0.045
_exptl_crystal_size_min          0.044
_refine_diff_density_max         0.701
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         2207
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0421
_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^)+(0.0853P)^2^+1.1250P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1172
_refine_ls_wR_factor_ref         0.1251
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2004
_reflns_number_total             2207
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt04368d2.cif
_cod_data_source_block           kcb38-44-12abs
_cod_depositor_comments
'Adding full bibliography for 7710412--7710415.cif.'
_cod_database_code               7710413
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Zn1 C16 N2 F2 O4'
_chemical_oxdiff_usercomment     'Zn fan 4,4 bpy from MeOH H2O'
_reflns_odcompleteness_completeness 99.38
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.62
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C10(H10), C11(H11), C9(H9), C17(H17), C15(H15), C18(H18), C16(H16)
;
_shelx_res_checksum              96654
_shelx_hkl_checksum              88760
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.547
_oxdiff_exptl_absorpt_empirical_full_min 0.741