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_7710412
_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 Fe N4 O4'
_chemical_formula_sum            'C26 H16 F2 Fe N4 O4'
_chemical_formula_weight         542.28
_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                 97.4780(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.84790(10)
_cell_length_b                   9.60960(10)
_cell_length_c                   16.33170(10)
_cell_measurement_reflns_used    8666
_cell_measurement_temperature    100.2(6)
_cell_measurement_theta_max      77.7220
_cell_measurement_theta_min      5.3480
_cell_volume                     2154.82(3)
_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      N~2~
_diffrn_ambient_temperature      100.2(6)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.975
_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    -44.00 -10.00   0.50    0.79    --  -48.30  38.00 -30.00   68
  2  \w    -39.00  20.00   0.50    0.79    --  -48.30  38.00  30.00  118
  3  \w    -28.00  24.00   0.50    0.79    --  -48.30  38.00  90.00  104
  4  \w    -49.00 -21.00   0.50    3.16    --  -86.25  45.00 -60.00   56
  5  \w    -20.00  22.00   0.50    0.79    --  -48.30  19.00-120.00   84
  6  \w    -69.00 -16.00   0.50    3.16    --  -86.25  61.00  30.00  106
  7  \w    -47.00 -15.00   0.50    3.16    --  -86.25  61.00 120.00   64
  8  \w   -132.00 -91.00   0.50    3.16    --  -86.25 -94.00  30.00   82
  9  \w   -103.00 -73.00   0.50    0.79    --  -48.30-125.00 -60.00   60
 10  \w   -158.00 -75.00   0.50    3.16    --  -86.25 -45.00 -60.00  166
 11  \w    -29.00  14.00   0.50    0.79    --  -48.30  19.00-180.00   86
 12  \w     68.00  93.00   0.50    3.16    --  107.75 -94.00-120.00   50
 13  \w     73.00 104.00   0.50    3.16    --  107.75 -94.00-180.00   62
 14  \w     64.00  90.00   0.50    3.16    --  107.75 -77.00 -90.00   52
 15  \w     69.00 105.00   0.50    3.16    --  107.75 -94.00 -90.00   72
 16  \w     80.00 106.00   0.50    3.16    --  107.75-125.00   0.00   52
 17  \w     70.00 100.00   0.50    3.16    --  107.75 -94.00   0.00   60
 18  \w     62.00  88.00   0.50    3.16    --  107.75 -77.00   0.00   52
 19  \w     36.00  69.00   0.50    3.16    --  107.75 -61.00 -30.00   66
 20  \w     41.00  67.00   0.50    3.16    --  107.75 -94.00   0.00   52
 21  \w     36.00  68.00   0.50    3.16    --  107.75 -61.00  30.00   64
 22  \w     62.00 106.00   0.50    3.16    --  107.75 -94.00  90.00   88
 23  \w     50.00  92.00   0.50    0.79    --   48.30-125.00 150.00   84
 24  \w     36.00 106.00   0.50    3.16    --  107.75-125.00 120.00  140
 25  \w     36.00  61.00   0.50    3.16    --  107.75 -61.00 120.00   50
 26  \w     39.00  68.00   0.50    3.16    --  107.75 -61.00 150.00   58
 27  \w     38.00  98.00   0.50    3.16    --  107.75 -77.00 150.00  120
 28  \w     97.00 168.00   0.50    3.16    --  107.75  45.00 120.00  142
 29  \w    134.00 178.00   0.50    3.16    --  107.75  77.00  30.00   88
 30  \w    140.00 178.00   0.50    3.16    --  107.75  45.00 -60.00   76
 31  \w    111.00 174.00   0.50    3.16    --  107.75  61.00-180.00  126
 32  \w    106.00 165.00   0.50    3.16    --  107.75  45.00-150.00  118
 33  \w     97.00 126.00   0.50    3.16    --  107.75  45.00 -60.00   58
 34  \w     37.00  76.00   0.50    3.16    --  107.75 -77.00-120.00   78
 35  \w     39.00  65.00   0.50    3.16    --  107.75 -94.00-120.00   52
 36  \w   -116.00 -91.00   0.50    0.79    --  -48.30-125.00 150.00   50
;
_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      0.0394468000
_diffrn_orient_matrix_UB_12      -0.1407759000
_diffrn_orient_matrix_UB_13      0.0348980000
_diffrn_orient_matrix_UB_21      -0.1029250000
_diffrn_orient_matrix_UB_22      -0.0628994000
_diffrn_orient_matrix_UB_23      -0.0177695000
_diffrn_orient_matrix_UB_31      0.0209948000
_diffrn_orient_matrix_UB_32      -0.0438450000
_diffrn_orient_matrix_UB_33      -0.0867046000
_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  0.0261
_diffrn_reflns_av_unetI/netI     0.0181
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11214
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.909
_diffrn_reflns_theta_min         5.353
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.173
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.817
_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            black
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_description       block
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.115
_exptl_crystal_size_mid          0.092
_exptl_crystal_size_min          0.049
_refine_diff_density_max         0.265
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         2246
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0273
_refine_ls_R_factor_gt           0.0271
_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^)+(0.0365P)^2^+2.3689P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0740
_refine_ls_wR_factor_ref         0.0741
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2217
_reflns_number_total             2246
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt04368d2.cif
_cod_data_source_block           kca038_167_6_meoh2-absxx
_cod_depositor_comments
'Adding full bibliography for 7710412--7710415.cif.'
_cod_database_code               7710412
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_chemical_oxdiff_usercomment     'Fe H2Fan MePyrV in MeOH and water'
_reflns_odcompleteness_completeness 100.00
_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:
 C00B(H00B), C00C(H00C), C00D(H00D), C00F(H00F), C00G(H00G), C00H(H00H),
 C00I(H00I), C00J(H00J)
;
_shelx_res_checksum              94778
_shelx_hkl_checksum              17411
_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 1.370
_oxdiff_exptl_absorpt_empirical_full_min 0.845