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_7049350
_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_absolute_configuration rmad
_chemical_formula_moiety         '2(C16.5 H16.5 B Br2 Fe0.5 N3 O3), 1[CH2Cl2]'
_chemical_formula_sum            'C33 H33 B2 Br4 Fe N6 O6'
_chemical_formula_weight         1006.76
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-10-25
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.0642(6)
_cell_length_b                   17.8345(8)
_cell_length_c                   16.9600(8)
_cell_measurement_reflns_used    8611
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      30.4010
_cell_measurement_theta_min      2.9280
_cell_volume                     4254.0(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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 10.5633
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.934
_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    -54.00  14.00   1.00   38.31    --   19.91 -38.00 -90.00   68
  2  \w    -12.00  96.00   1.00   38.31    --   19.91  77.00  60.00  108
  3  \w   -107.00 -67.00   1.00   38.31    --  -20.22 178.00-180.00   40
  4  \w    -87.00 -13.00   1.00   38.31    --  -20.22 -38.00 -60.00   74
  5  \w    -28.00  48.00   1.00   38.31    --  -20.22  57.00-150.00   76
  6  \w    -65.00  12.00   1.00   38.31    --  -20.22 -77.00 120.00   77
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0366094000
_diffrn_orient_matrix_UB_12      -0.0107206000
_diffrn_orient_matrix_UB_13      -0.0263455000
_diffrn_orient_matrix_UB_21      -0.0326267000
_diffrn_orient_matrix_UB_22      -0.0018523000
_diffrn_orient_matrix_UB_23      0.0319267000
_diffrn_orient_matrix_UB_31      -0.0117435000
_diffrn_orient_matrix_UB_32      0.0382548000
_diffrn_orient_matrix_UB_33      -0.0060203000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0686
_diffrn_reflns_av_unetI/netI     0.0723
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.934
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            56046
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.910
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.065
_diffrn_reflns_theta_min         2.581
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.158
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.074
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (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 red'
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_description       plate
_exptl_crystal_F_000             1988
_exptl_crystal_size_max          0.719
_exptl_crystal_size_mid          0.524
_exptl_crystal_size_min          0.199
_refine_diff_density_max         0.955
_refine_diff_density_min         -0.999
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.20(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         14690
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1377
_refine_ls_R_factor_gt           0.0680
_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^)+(0.0739P)^2^+4.1503P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1659
_refine_ls_wR_factor_ref         0.2005
_reflns_Friedel_coverage         0.790
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.882
_reflns_number_gt                7740
_reflns_number_total             14690
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00546c2.cif
_cod_data_source_block           jb-425
_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        4254.1(3)
_cod_database_code               7049350
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C33 H39 B2 N6 O6 Fe1 Br4'
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.80(2)
 0.20(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C11B-C8 = C26A-C25 = C26B-C24 = C3-C4 = C20-C21
 1.54 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
N2 \\sim N3 \\sim C5 \\sim C6 \\sim C11A \\sim C11B \\sim N6 \\sim C26A \\sim
C26B \\sim C27: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
5. Others
 Sof(H9A)=Sof(H9B)=Sof(C11B)=Sof(H11D)=Sof(H11E)=Sof(H11F)=1-FVAR(1)
 Sof(H8A)=Sof(H8B)=Sof(C11A)=Sof(H11A)=Sof(H11B)=Sof(H11C)=FVAR(1)
 Sof(HJ)=Sof(HK)=Sof(C26B)=Sof(HO)=Sof(HP)=Sof(HQ)=1-FVAR(2)
 Sof(HH)=Sof(HI)=Sof(C26A)=Sof(HL)=Sof(HM)=Sof(HN)=FVAR(2)
 Fixed Sof: C4(0.5) H4A(0.5) H4B(0.5) H4C(0.5) C21(0.5) HC(0.5) HD(0.5) HE(0.5)
6.a Ternary CH refined with riding coordinates:
 C3(H3), C20(HB)
6.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C19(H,HA),
  C23(HF,HG), C24(HH,HI), C25(HJ,HK), C28(HR,HS)
6.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C15(H15), C17(H17), C30(HT), C32(HU), C34(HV)
6.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C11A(H11A,H11B,H11C), C11B(H11D,H11E,H11F), C21(HC,HD,HE),
 C26A(HL,HM,HN), C26B(HO,HP,HQ)
;
_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 1.778
_oxdiff_exptl_absorpt_empirical_full_min 0.515