Large, heterometallic coordination cages based on ditopic metallo-ligands with 3-pyridyl donor groups
Wise, Matthew D.; Holstein, Julian J.; Pattison, Philip; Besnard, Celine; Solari, Euro; Scopelliti, Rosario; Bricogne, Gerard; Severin, Kay; Chem. Sci. 6 (2015) 1004–; doi:10.1039/C4SC03046J

data_1518252
_publ_section_title
;
 Large, heterometallic coordination cages based on ditopic metallo-ligands
 with 3-pyridyl donor groups
;
_journal_issue                   2
_journal_name_full               'Chem. Sci.'
_journal_page_first              1004
_journal_paper_doi               10.1039/C4SC03046J
_journal_volume                  6
_journal_year                    2015
_chemical_formula_moiety         'C22 H26 B2 Fe N8 O6, 2(C H Cl3)'
_chemical_formula_sum            'C24 H28 B2 Cl6 Fe N8 O6'
_chemical_formula_weight         814.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 120.269(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.287(3)
_cell_length_b                   8.1945(5)
_cell_length_c                   20.3960(18)
_cell_measurement_reflns_used    2691
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.1228
_cell_measurement_theta_min      3.6571
_cell_volume                     3505.8(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics    'shelXle (Huebschle, 2014)'
_computing_publication_material  'enCIFer 1.3, CCDC, 2008'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SIR2011 (Giacovazzo, 2011)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 10.2665
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0720013000
_diffrn_orient_matrix_UB_12      0.0213427000
_diffrn_orient_matrix_UB_13      -0.0303068000
_diffrn_orient_matrix_UB_21      0.0122945000
_diffrn_orient_matrix_UB_22      -0.0095694000
_diffrn_orient_matrix_UB_23      0.0818033000
_diffrn_orient_matrix_UB_31      0.0087478000
_diffrn_orient_matrix_UB_32      0.1861301000
_diffrn_orient_matrix_UB_33      0.0075670000
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_unetI/netI     0.0524
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6161
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         73.272
_diffrn_reflns_theta_min         4.215
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.090
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.02384
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_description       needle
_exptl_crystal_F_000             1656
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: CDCl3'
_exptl_crystal_size_max          0.808
_exptl_crystal_size_mid          0.182
_exptl_crystal_size_min          0.165
_refine_diff_density_max         0.703
_refine_diff_density_min         -0.615
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       0.00039(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.796
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         3405
_refine_ls_number_restraints     88
_refine_ls_restrained_S_all      0.799
_refine_ls_R_factor_all          0.0735
_refine_ls_R_factor_gt           0.0610
_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^)+(0.1175P)^2^+16.6454P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1593
_refine_ls_wR_factor_ref         0.1741
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2855
_reflns_number_total             3405
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4sc03046j2.cif
_cod_data_source_block           ligand1
_cod_depositor_comments
'Adding full bibliography for 1518252--1518257.cif.'
_cod_database_code               1518252
_shelx_estimated_absorpt_t_min   0.059
_shelx_estimated_absorpt_t_max   0.349
_computing_refinement_gui        'shelXle (Huebschle, 2014)'
_shelxl_version_number           2014/6
_shelx_res_checksum              70446