Carboxylic Acid Functionalized Clathrochelate Complexes: Large, Robust, and Easy-to-Access Metalloligands.
Marmier, Mathieu; Wise, Matthew D.; Holstein, Julian J.; Pattison, Philip; Schenk, Kurt; Solari, Euro; Scopelliti, Rosario; Severin, Kay; Inorganic chemistry 55 (2016) 4006–4015; doi:10.1021/acs.inorgchem.6b00276

data_4347520
_publ_section_title
;
 Carboxylic Acid Functionalized Clathrochelate Complexes: Large, Robust,
 and Easy-to-Access Metalloligands.
;
_journal_issue                   8
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4006
_journal_page_last               4015
_journal_paper_doi               10.1021/acs.inorgchem.6b00276
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         '3(C50 H47 B6 Co6 N6 O13) (O2 ZN4)'
_chemical_formula_sum            'C150 H141 B6 Co6 N18 O41 Zn4'
_chemical_formula_weight         3531.72
_space_group_crystal_system      trigonal
_space_group_IT_number           166
_space_group_name_Hall           '-R 3 2"'
_space_group_name_H-M_alt        'R -3 m :H'
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_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   31.837(8)
_cell_length_b                   31.837(8)
_cell_length_c                   62.41(2)
_cell_measurement_reflns_used    36
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      3
_cell_volume                     54783(3)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs, 1990-2000)'
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_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2496
_diffrn_reflns_av_unetI/netI     0.1000
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            33033
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        15.872
_diffrn_reflns_theta_max         15.872
_diffrn_reflns_theta_min         1.279
_exptl_absorpt_coefficient_mu    0.559
_exptl_absorpt_correction_T_max  0.6979
_exptl_absorpt_correction_T_min  0.4316
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008, Bruker AXS, 2008'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    0.642
_exptl_crystal_description       prism
_exptl_crystal_F_000             10842
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_exptl_crystal_size_mid          0.269
_exptl_crystal_size_min          0.150
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_refine_diff_density_min         -0.694
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         3173
_refine_ls_number_restraints     1447
_refine_ls_restrained_S_all      1.150
_refine_ls_R_factor_all          0.1677
_refine_ls_R_factor_gt           0.1038
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2752
_refine_ls_wR_factor_ref         0.3461
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1786
_reflns_number_total             3173
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00276_si_006.cif
_cod_data_source_block           mof18
_cod_original_cell_volume        54787(34)
_cod_database_code               4347520
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.852
_shelx_estimated_absorpt_t_max   0.921
_computing_refinement_gui        'shelXle (Huebschle, 2014)'
_computing_ligand_restraints
'Grade Web Server, http://grade.globalphasing.org'
_computing_molecular_model       'DSR (Kratzert, 2015)'
_shelx_res_checksum              45492
_shelx_hkl_checksum              65490
_shelx_fab_checksum              38802