A family of tri- and dimetallic pyridine dicarboxamide cryptates: unusual o,n,o-coordination and facile access to secondary coordination sphere hydrogen bonding interactions.
Guillet, Gary L.; Gordon, Jesse B.; Di Francesco, Gianna N.; Calkins, Matthew W.; Čižmár, Erik; Abboud, Khalil A.; Meisel, Mark W.; García-Serres, Ricardo; Murray, Leslie J.; Inorganic chemistry 54 (2015) 2691–2704; doi:10.1021/ic502873d

data_4342506
_publ_section_title
;
 A family of tri- and dimetallic pyridine dicarboxamide cryptates: unusual
 o,n,o-coordination and facile access to secondary coordination sphere
 hydrogen bonding interactions.
;
_journal_issue                   6
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2691
_journal_page_last               2704
_journal_paper_doi               10.1021/ic502873d
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety
'C93 H104 N10 O20 F6 S2 Co3, 2(CF3SO3), (C4H8O1), 4(C2H3N1)'
_chemical_formula_sum            'C111 H118 Co3 F12 N14 O26 S4'
_chemical_formula_weight         2597.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2014-05-22 # Formatted by publCIF

;
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_cell_length_c                   23.8572(6)
_cell_measurement_reflns_used    4781
_cell_measurement_temperature    100(2)
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_cell_measurement_theta_min      2.0
_cell_volume                     12295.7(5)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2 (Bruker, 2008)'
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_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.686
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker APEX-II DUO'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           CuK\a
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_diffrn_reflns_Laue_measured_fraction_full 0.686
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_diffrn_reflns_limit_h_max       11
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_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
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_diffrn_reflns_number            46558
_diffrn_reflns_point_group_measured_fraction_full 0.686
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_diffrn_source                   'I\mS microsource'
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_exptl_absorpt_correction_T_min  0.2151
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
'based on measured indexed crystal faces, Bruker SHELXTL  v6.14 (Bruker 2008)'
_exptl_crystal_colour            yellow
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_exptl_crystal_description       plates
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_refine_diff_density_max         0.732
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         15263
_refine_ls_number_restraints     65
_refine_ls_restrained_S_all      0.884
_refine_ls_R_factor_all          0.1736
_refine_ls_R_factor_gt           0.0948
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2181
_refine_ls_wR_factor_ref         0.2451
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5839
_reflns_number_total             15263
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic502873d_si_003.cif
_cod_data_source_block           gui28
_cod_depositor_comments
'Adding full bibliography for 4342504--4342510.cif.'
_cod_database_code               4342506
_shelx_estimated_absorpt_t_min   0.638
_shelx_estimated_absorpt_t_max   0.947
_shelxl_version_number           2013-3
_shelx_res_checksum              7531
_shelx_hkl_checksum              1697