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_4347518
_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
'2(C153 H146 B6 N19 O42 Zn10), 2(C8 H20 N), C2 H8 N'
_chemical_formula_sum            'C324 H340 B12 N41 O84 Zn20'
_chemical_formula_weight         7589.47
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
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_atom_sites_solution_hydrogens   geom
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_cell_angle_beta                 91.5280(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   35.8409(2)
_cell_length_b                   42.7516(2)
_cell_length_c                   50.8130(5)
_cell_measurement_reflns_used    15891
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.3650
_cell_measurement_theta_min      2.0871
_cell_volume                     77830.8(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection       'Pylatus software, SNBL@ESRF (Dyadkin 2013)'
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_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    'SUPERFLIP(Palatinus et al., 2007)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
'Pilatus 2M, Dectris-CrysAlisPro-abstract goniometer imported dectris images'
_diffrn_measurement_method       '\p scans'
_diffrn_radiation_type           synchrotron
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_diffrn_reflns_av_R_equivalents  0.0527
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_Laue_measured_fraction_full 0.997
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_diffrn_reflns_limit_h_max       35
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_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            229579
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        20.375
_diffrn_reflns_theta_max         20.375
_diffrn_reflns_theta_min         1.453
_diffrn_source
'Swiss Norwegian beamline @ ESRF, Grenoble, France'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.641
_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            yellow
_exptl_crystal_density_diffrn    0.648
_exptl_crystal_description       prism
_exptl_crystal_F_000             15612
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.300
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_refine_diff_density_min         -0.695
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2628
_refine_ls_number_reflns         40637
_refine_ls_number_restraints     7798
_refine_ls_restrained_S_all      1.964
_refine_ls_R_factor_all          0.1192
_refine_ls_R_factor_gt           0.1118
_refine_ls_shift/su_max          0.001
_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^-0.0550P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4136
_refine_ls_wR_factor_ref         0.4229
_reflns_Friedel_coverage         0.000
_reflns_number_gt                34931
_reflns_number_total             40637
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00276_si_005.cif
_cod_data_source_block           mof17
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4347518
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.784
_shelx_estimated_absorpt_t_max   0.831
_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              93758
_shelx_hkl_checksum              29312
_shelx_fab_checksum              91320