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_4347521
_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         '(C28 H32 B2 Fe N6 O10) (N O C4 H9) Zn'
_chemical_formula_sum            'C36 H41 B2 Fe N7 O11 Zn'
_chemical_formula_weight         890.60
_space_group_crystal_system      monoclinic
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_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
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_cell_angle_gamma                90
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_cell_length_b                   24.173(6)
_cell_length_c                   19.292(6)
_cell_measurement_reflns_used    174
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      3
_cell_volume                     10342(6)
_computing_cell_refinement       'automar, marresearch, 2010'
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'marmux - Micro-beam system, marresearch, 2010'
_computing_data_reduction        'automar, marresearch, 2010'
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_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      140(2)
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_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_unetI/netI     0.0667
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_diffrn_reflns_theta_max         22.203
_diffrn_reflns_theta_min         2.068
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.797
_exptl_absorpt_correction_T_max  0.863
_exptl_absorpt_correction_T_min  0.826
_exptl_absorpt_correction_type   semi-empirical
_exptl_absorpt_process_details   'SADABS 2008, Bruker AXS, 2008'
_exptl_crystal_colour            red
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_exptl_crystal_description       prism
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_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
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_refine_ls_number_reflns         6369
_refine_ls_number_restraints     1004
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0873
_refine_ls_R_factor_gt           0.0664
_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^)+(0.1374P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1852
_refine_ls_wR_factor_ref         0.2002
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4365
_reflns_number_total             6369
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00276_si_009.cif
_cod_data_source_block           mof21
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4347521
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.826
_shelx_estimated_absorpt_t_max   0.863
_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              14661
_shelx_hkl_checksum              88761
_shelx_fab_checksum              96685