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_4347525
_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         'C50 H49 B2 Co2 N6 O13, C8 H20 N, 0.5(C7 H8)'
_chemical_formula_sum            'C61.5 H73 B2 Co2 N7 O13'
_chemical_formula_weight         1257.74
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-12-07 # Formatted by publCIF

;
_cell_angle_alpha                79.278(12)
_cell_angle_beta                 77.959(13)
_cell_angle_gamma                62.972(11)
_cell_formula_units_Z            4
_cell_length_a                   16.359(2)
_cell_length_b                   16.504(2)
_cell_length_c                   32.228(6)
_cell_measurement_reflns_used    210
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      3
_cell_volume                     7539(2)
_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    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0669
_diffrn_reflns_av_unetI/netI     0.1179
_diffrn_reflns_Laue_measured_fraction_full 0.954
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            66550
_diffrn_reflns_point_group_measured_fraction_full 0.954
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        24.800
_diffrn_reflns_theta_max         24.800
_diffrn_reflns_theta_min         1.494
_exptl_absorpt_coefficient_mu    0.496
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.4867
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008, Bruker AXS, 2008'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.108
_exptl_crystal_description       prism
_exptl_crystal_F_000             2636
_exptl_crystal_size_max          0.459
_exptl_crystal_size_mid          0.302
_exptl_crystal_size_min          0.296
_refine_diff_density_max         1.004
_refine_diff_density_min         -0.817
_refine_diff_density_rms         0.116
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.45(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3020
_refine_ls_number_reflns         41354
_refine_ls_number_restraints     5589
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1252
_refine_ls_R_factor_gt           0.0953
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1568P)^2^+9.0677P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2407
_refine_ls_wR_factor_ref         0.2661
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.954
_reflns_Friedel_fraction_max     0.954
_reflns_number_gt                30609
_reflns_number_total             41354
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00276_si_001.cif
_cod_data_source_block           shelx
_cod_original_formula_sum        'C61.50 H73 B2 Co2 N7 O13'
_cod_database_code               4347525
_publcif_datablock.id            {7bec26c7-29ad-4b63-af73-8dbe3e520835}
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.804
_shelx_estimated_absorpt_t_max   0.867
_shelx_res_checksum              94927
_shelx_hkl_checksum              24184
_shelx_fab_checksum              57033
_publcif_info_exptl_table_max_cols 4
_publcif_info_exptl_table_use_headnotes n