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_4347522
_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         'C32 H34 B2 Fe N6 O10, 3(C2 H6 O S)'
_chemical_formula_sum            'C38 H52 B2 Fe N6 O13 S3'
_chemical_formula_weight         974.50
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 93.90(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.950(4)
_cell_length_b                   22.639(5)
_cell_length_c                   10.833(2)
_cell_measurement_reflns_used    128
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      3
_cell_volume                     4881.4(17)
_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)'
_computing_molecular_graphics    'shelXle (Huebschle, 2014)'
_computing_publication_material  'enCIFer 1.3, CCDC, 2008'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphit
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1373
_diffrn_reflns_av_unetI/netI     0.0766
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            38979
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        12.500
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         3.200
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.501
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5926
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008, Bruker AXS, 2008'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_description       prism
_exptl_crystal_F_000             2040
_exptl_crystal_size_max          0.407
_exptl_crystal_size_mid          0.128
_exptl_crystal_size_min          0.062
_refine_diff_density_max         0.953
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         4292
_refine_ls_number_restraints     157
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.1105
_refine_ls_R_factor_gt           0.0734
_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^)+(0.0510P)^2^+35.9726P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1617
_refine_ls_wR_factor_ref         0.1763
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3112
_reflns_number_total             4292
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00276_si_002.cif
_cod_data_source_block           ligand6
_cod_original_cell_volume        4881.5(17)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4347522
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.822
_shelx_estimated_absorpt_t_max   0.970
_computing_refinement_gui        'shelXle (Huebschle, 2014)'
_shelx_res_checksum              28772
_shelx_hkl_checksum              76700
_shelx_fab_checksum              63068