Porous networks based on iron(ii) clathrochelate complexes.
Bila, José L; Pijeat, Joffrey; Ramorini, Andrea; Fadaei-Tirani, Farzaneh; Scopelliti, Rosario; Baudat, Emilie; Severin, Kay; Dalton transactions (Cambridge, England : 2003) 48 (2019) 4582–4588; doi:10.1039/c9dt00546c

data_7049348
_publ_section_title
;
 Porous networks based on iron(ii) clathrochelate complexes.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4582
_journal_page_last               4588
_journal_paper_doi               10.1039/c9dt00546c
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C28 H28 B2 Fe N6 O6'
_chemical_formula_sum            'C28 H28 B2 Fe N6 O6'
_chemical_formula_weight         622.03
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-10-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-11-04 deposited with the CCDC.    2019-03-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.090(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8991(2)
_cell_length_b                   16.1046(3)
_cell_length_c                   16.9882(3)
_cell_measurement_reflns_used    9623
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      75.8860
_cell_measurement_theta_min      3.8030
_cell_volume                     2892.15(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2817
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.977
_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    -65.00  27.00   1.00    2.50    --  -40.91  38.00 -60.00   92
  2  \w   -112.00 -16.00   1.00    2.50    --  -40.91 -38.00 120.00   96
  3  \w    -69.00  32.00   1.00    2.50    --  -40.91  57.00  30.00  101
  4  \w     57.00  89.00   1.00    2.50    --   40.91-125.00 -90.00   32
  5  \w      9.00  81.00   1.00    2.50    --   40.91 -99.00  90.00   72
  6  \w     17.00  44.00   1.00    2.50    --   40.91  38.00 -60.00   27
  7  \w     91.00 117.00   1.00    2.50    --   40.91  77.00-120.00   26
  8  \w     41.00 137.00   1.00   10.00    --  112.00 -30.00-150.00   96
  9  \w     30.00 164.00   1.00   10.00    --  112.00 -15.00  30.00  134
 10  \w     86.00 178.00   1.00   10.00    --  112.00  45.00  30.00   92
 11  \w     90.00 118.00   1.00   10.00    --  112.00-125.00  30.00   28
 12  \w     40.00 134.00   1.00   10.00    --  112.00 -61.00  90.00   94
 13  \w     32.00 109.00   1.00   10.00    --  112.00 -94.00  60.00   77
 14  \w     88.00 118.00   1.00   10.00    --  112.00-125.00-150.00   30
 15  \w    101.00 126.00   1.00   10.00    --  112.00 125.00-180.00   25
 16  \w     40.00 114.00   1.00   10.00    --  112.00-125.00 -90.00   74
 17  \w     53.00  98.00   1.00   10.00    --  112.00 -30.00   0.00   45
 18  \w     44.00 145.00   1.00   10.00    --  112.00 -77.00-120.00  101
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1112245000
_diffrn_orient_matrix_UB_12      0.0168062000
_diffrn_orient_matrix_UB_13      0.0391144000
_diffrn_orient_matrix_UB_21      0.0823639000
_diffrn_orient_matrix_UB_22      -0.0276977000
_diffrn_orient_matrix_UB_23      0.0828768000
_diffrn_orient_matrix_UB_31      0.0461290000
_diffrn_orient_matrix_UB_32      0.0899593000
_diffrn_orient_matrix_UB_33      0.0182245000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0610
_diffrn_reflns_av_unetI/netI     0.0513
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18388
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.244
_diffrn_reflns_theta_min         3.838
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.631
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.022
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
 Numerical absorption correction based on Gaussian integration over
 a multifaceted crystal model/Empirical absorption correction using
 spherical harmonics, as implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear intense orange'
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_description       plate
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.76
_exptl_crystal_size_mid          0.604
_exptl_crystal_size_min          0.036
_refine_diff_density_max         0.834
_refine_diff_density_min         -0.939
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         5928
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0603
_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^)+(0.1313P)^2^+0.0629P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1700
_refine_ls_wR_factor_ref         0.1762
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5407
_reflns_number_total             5928
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00546c2.cif
_cod_data_source_block           ara-13
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Gaussian' changed to
'gaussian' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

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

 Adding full bibliography for 7049348--7049350.cif.
;
_cod_original_cell_volume        2892.17(10)
_cod_database_code               7049348
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C28 H28 B2 Fe N6 O6'
_reflns_odcompleteness_completeness 99.42
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C17(H17), C18(H18), C22(H22), C23(H23), C25(H25), C26(H26)
2.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C11(H11A,
 H11B,H11C), C12(H12A,H12B,H12C)
2.c :
 C20(H20), C28(H28)
;
_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
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 6.748
_oxdiff_exptl_absorpt_empirical_full_min 0.452