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_7049349
_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         'C34 H34 B2 Fe N6 O6, 0.5[CH2Cl2]'
_chemical_formula_sum            'C34 H34 B2 Fe N6 O6'
_chemical_formula_weight         700.14
_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'
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-10-31
_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                 97.269(3)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   30.5087(8)
_cell_length_b                   9.8259(2)
_cell_length_c                   46.0071(17)
_cell_measurement_reflns_used    12206
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      74.2790
_cell_measurement_theta_min      4.5260
_cell_volume                     13681.0(7)
_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      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2665
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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    -70.00  25.00   0.50   10.00    --  -43.01  57.00  60.00  190
  2  \w   -106.00 -19.00   0.50   10.00    --  -43.01 -37.00 150.00  174
  3  \w    -67.00  31.00   0.50   10.00    --  -43.01  37.00 -30.00  196
  4  \w   -122.00 -95.00   0.50   10.00    --  -43.01 -99.00 -60.00   54
  5  \w      2.00  84.00   0.50   10.00    --   43.01 -99.00 150.00  164
  6  \w     98.00 169.00   0.50   40.00    --  109.26  45.00 -60.00  142
  7  \w     54.00 113.00   0.50   40.00    --  109.26-111.00-120.00  118
  8  \w     50.00 135.00   0.50   40.00    --  109.26 -45.00  60.00  170
  9  \w    109.00 136.00   0.50   40.00    --  109.26 111.00-120.00   54
 10  \w    100.00 173.00   0.50   40.00    --  109.26 111.00 150.00  146
 11  \w     74.00 101.00   0.50   40.00    --  109.26-111.00 -60.00   54
 12  \w     38.00 113.00   0.50   40.00    --  109.26-111.00 120.00  150
 13  \w     81.00 172.00   0.50   40.00    --  109.26  30.00-120.00  182
 14  \w     65.00 113.00   0.50   40.00    --  109.26-111.00   0.00   96
 15  \w     72.00 137.00   0.50   40.00    --  109.26 -77.00 120.00  130
 16  \w    100.00 161.00   0.50   40.00    --  109.26 111.00 120.00  122
 17  \w     36.00 125.00   0.50   40.00    --  109.26 -45.00-150.00  178
 18  \w     95.00 164.00   0.50   40.00    --  109.26 146.00 171.00  138
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0508887000
_diffrn_orient_matrix_UB_12      -0.0012727000
_diffrn_orient_matrix_UB_13      -0.0032924000
_diffrn_orient_matrix_UB_21      -0.0015224000
_diffrn_orient_matrix_UB_22      0.0193830000
_diffrn_orient_matrix_UB_23      -0.0333470000
_diffrn_orient_matrix_UB_31      0.0002294000
_diffrn_orient_matrix_UB_32      -0.1555428000
_diffrn_orient_matrix_UB_33      -0.0041335000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            44155
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        63.685
_diffrn_reflns_theta_max         63.685
_diffrn_reflns_theta_min         3.704
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.979
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.454
_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 red'
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_description       prism
_exptl_crystal_F_000             5824
_exptl_crystal_size_max          0.867
_exptl_crystal_size_mid          0.116
_exptl_crystal_size_min          0.056
_refine_diff_density_max         1.281
_refine_diff_density_min         -0.833
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1000
_refine_ls_number_reflns         11115
_refine_ls_number_restraints     1384
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.1281
_refine_ls_R_factor_gt           0.1170
_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^)+(0.1648P)^2^+154.0936P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3284
_refine_ls_wR_factor_ref         0.3377
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9347
_reflns_number_total             11115
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00546c2.cif
_cod_data_source_block           ara-12
_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_database_code               7049349
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C34 H34 B2 Fe N6 O6'
_reflns_odcompleteness_completeness 98.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 C26-C25
 1.17 with sigma of 0.01
 N8-C36 = N1-C1 = N6-C14 = N4-C12 = N3-C7
 1.33 with sigma of 0.01
 C62B-C61 = C66B-C61 = C65B-C66B = C65B-C64 = C63B-C64 = C62B-C63B
 1.39 with sigma of 0.005
 N11-C47A \\sim N11-C47B \\sim N12-C48A \\sim N12-C48B
 with sigma of 0.01
 C47A-C48A \\sim C48B-C47B
 with sigma of 0.01
 C52A-C47A \\sim C51A-C52A \\sim C51A-C50A \\sim C49A-C50A \\sim C49A-C48A
\\sim C52B-C47B \\sim C52B-
 C51B \\sim C50B-C51B \\sim C50B-C49B \\sim C48B-C49B
 with sigma of 0.01
 C17A-C18 \\sim C17B-C18 \\sim C16A-C15 \\sim C16B-C15
 with sigma of 0.01
 C17A-C16A \\sim C17B-C16B
 with sigma of 0.01
 C67A-C64 \\sim C67B-C64
 with sigma of 0.01
 C68A-C67A \\sim C67B-C68B
 with sigma of 0.01
 C68A-C64 \\sim C64-C68B
 with sigma of 0.005
 C63B-C68B \\sim C68B-C65B
 with sigma of 0.02
 C65A-C68A \\sim C68A-C63A
 with sigma of 0.02
3. Restrained planarity
 C19, C20, C21, C22, C23, C24, C25, C26
 with sigma of 0.1
 C27, C28, C29, C30, C31, C32, C33, C34
 with sigma of 0.1
 C61, C62B, C63B, C64, C65B, C66B, C67B, C68B
 with sigma of 0.01
 C61, C62A, C63A, C64, C65A, C66A, C67A, C68A
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C16A \\sim C16B \\sim C17A \\sim C17B: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
C61 \\sim C62A \\sim C62B \\sim C63A \\sim C63B \\sim C64 \\sim C65A \\sim C65B
\\sim C66A \\sim C66B \\sim C67A \\sim C67B \\sim C68A \\sim C68B: within 2A
with sigma of 0.005 and sigma for terminal atoms of 0.01
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C47B)=Sof(C48B)=Sof(C49B)=Sof(H49C)=Sof(H49D)=Sof(C50B)=Sof(H50C)=
 Sof(H50D)=Sof(C51B)=Sof(H51C)=Sof(H51D)=Sof(C52B)=Sof(H52C)=Sof(H52D)=1-FVAR(1)
 Sof(C47A)=Sof(C48A)=Sof(C49A)=Sof(H49A)=Sof(H49B)=Sof(C50A)=Sof(H50A)=
 Sof(H50B)=Sof(C51A)=Sof(H51A)=Sof(H51B)=Sof(C52A)=Sof(H52A)=Sof(H52B)=FVAR(1)
 Sof(H15C)=Sof(H15D)=Sof(C16B)=Sof(H16C)=Sof(H16D)=Sof(C17B)=Sof(H17C)=
 Sof(H17D)=Sof(H18C)=Sof(H18D)=1-FVAR(2)
 Sof(H15A)=Sof(H15B)=Sof(C16A)=Sof(H16A)=Sof(H16B)=Sof(C17A)=Sof(H17A)=
 Sof(H17B)=Sof(H18A)=Sof(H18B)=FVAR(2)
 Sof(C62B)=Sof(H62B)=Sof(C63B)=Sof(H63B)=Sof(C65B)=Sof(H65B)=Sof(C66B)=
 Sof(H66B)=Sof(C67B)=Sof(C68B)=Sof(H68B)=1-FVAR(3)
 Sof(C66A)=Sof(H66A)=Sof(C65A)=Sof(H65A)=Sof(C63A)=Sof(H63A)=Sof(C62A)=
 Sof(H62A)=Sof(C67A)=Sof(C68A)=Sof(H68A)=FVAR(3)
7.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C8(H8A,H8B), C9(H9A,H9B),
 C10(H10A,H10B), C11(H11A,H11B), C15(H15A,H15B), C15(H15C,H15D), C16A(H16A,
 H16B), C16B(H16C,H16D), C17A(H17A,H17B), C17B(H17C,H17D), C18(H18A,H18B),
 C18(H18C,H18D), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B),
  C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C49A(H49A,
 H49B), C49B(H49C,H49D), C50A(H50A,H50B), C50B(H50C,H50D), C51A(H51A,H51B),
 C51B(H51C,H51D), C52A(H52A,H52B), C52B(H52C,H52D)
7.b Aromatic/amide H refined with riding coordinates:
 C20(H20), C21(H21), C23(H23), C24(H24), C28(H28), C29(H29), C31(H31),
 C32(H32), C54(H54), C55(H55), C57(H57), C58(H58), C66A(H66A), C65A(H65A),
 C63A(H63A), C62A(H62A), C62B(H62B), C63B(H63B), C65B(H65B), C66B(H66B)
7.c Fitted hexagon refined as free rotating group:
 C61(C66A,C65A,C64,C63A,C62A)
7.d :
 C26(H26), C34(H34), C60(H60), C68A(H68A), C68B(H68B)
;
_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 2.174
_oxdiff_exptl_absorpt_empirical_full_min 0.658