Large heterometallic coordination cages with gyrobifastigium-like geometry.
Cecot, Giacomo; Alameddine, Bassam; Prior, Stéphanie; Zorzi, Rita De; Geremia, Silvano; Scopelliti, Rosario; Fadaei, Farzaneh T.; Solari, Euro; Severin, Kay; Chemical communications (Cambridge, England) 52 (2016) 11243–11246; doi:10.1039/c6cc06066h

data_7124990
_publ_section_title
;
 Large heterometallic coordination cages with gyrobifastigium-like
 geometry.
;
_journal_issue                   75
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              11243
_journal_page_last               11246
_journal_paper_doi               10.1039/c6cc06066h
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C50 H52 B2 Fe N10 O6'
_chemical_formula_sum            'C50 H52 B2 Fe N10 O6'
_chemical_formula_weight         966.48
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-06-27
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-07-13 deposited with the CCDC.
2016-08-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.3120(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.84673(5)
_cell_length_b                   38.91135(19)
_cell_length_c                   14.15673(7)
_cell_measurement_reflns_used    18693
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      75.2830
_cell_measurement_theta_min      3.9460
_cell_volume                     4700.30(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5633
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.981
_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    -19.00  23.00   0.50    1.00    --  -40.91  38.00   0.00   84
  2  \w    -63.00  27.00   0.50    1.00    --  -40.91  57.00 -60.00  180
  3  \w    -65.00  29.00   0.50    1.00    --  -40.91  38.00-150.00  188
  4  \w     37.00  75.00   0.50    1.00    --   40.91 -99.00   0.00   76
  5  \w     39.00 139.00   0.50    4.00    --  110.60 -61.00-120.00  200
  6  \w     87.00 122.00   0.50    4.00    --  110.60-125.00 -30.00   70
  7  \w     80.00 136.00   0.50    4.00    --  110.60 -77.00 -60.00  112
  8  \w     86.00 129.00   0.50    4.00    --  110.60 -45.00 -30.00   86
  9  \w     85.00 173.00   0.50    4.00    --  110.60  30.00  60.00  176
 10  \w    144.00 170.00   0.50    4.00    --  110.60  30.00 150.00   52
 11  \w    114.00 140.00   0.50    4.00    --  110.60  30.00 150.00   52
 12  \w    112.00 139.00   0.50    4.00    --  110.60 -30.00 150.00   54
 13  \w     74.00 122.00   0.50    4.00    --  110.60-125.00 150.00   96
 14  \w     41.00  99.00   0.50    4.00    --  110.60 -30.00 150.00  116
 15  \w     86.00 177.00   0.50    4.00    --  110.60  45.00 -30.00  182
 16  \w    103.00 172.00   0.50    4.00    --  110.60 127.00 -78.00  138
 17  \w     96.00 157.00   0.50    4.00    --  110.60 125.00-120.00  122
 18  \w     38.00  67.00   0.50    4.00    --  110.60 -45.00 -30.00   58
 19  \w     37.00  96.00   0.50    4.00    --  110.60 -94.00-150.00  118
 20  \w     56.00  87.00   0.50    1.00    --   40.91-127.00-153.00   62
 21  \w   -113.00 -16.00   0.50    1.00    --  -40.91 -38.00  30.00  194
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_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  0.0229
_diffrn_reflns_av_unetI/netI     0.0199
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            33734
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         75.495
_diffrn_reflns_theta_min         3.430
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.078
_exptl_absorpt_correction_T_max  0.622
_exptl_absorpt_correction_T_min  0.314
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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            'clear intense red'
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2024
_exptl_crystal_size_max          0.698
_exptl_crystal_size_mid          0.291
_exptl_crystal_size_min          0.214
_refine_diff_density_max         0.371
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.042
_refine_ls_extinction_coef       0.00013(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     629
_refine_ls_number_reflns         9562
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0310
_refine_ls_R_factor_gt           0.0299
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0416P)^2^+1.7378P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0785
_refine_ls_wR_factor_ref         0.0794
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9221
_reflns_number_total             9562
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc06066h2.cif
_cod_data_source_block           gc2-ba1510
_cod_database_code               7124990
_olex2_refinement_description
;
1. 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
2.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C15(H15A,H15B), C19(H19A,H19B), C24(H24A,H24B), C37(H37A,
 H37B), C40(H40A,H40B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C5(H5), C6(H6), C10(H10), C16(H16), C17(H17), C18(H18), C22(H22),
 C26(H26), C29(H29), C30(H30), C33(H33), C34(H34), C35(H35), C36(H36), C38(H38),
  C43(H43), C44(H44), C45(H45), C46(H46), C47(H47), C49(H49)
2.c Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C), C42(H42A,H42B,
 H42C), C48(H48A,H48B,H48C), C50(H50A,H50B,H50C)
;
_shelx_res_checksum              21177
_shelx_hkl_checksum              39319
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'