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_4342507
_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_sum            'C113 H150.5 Cl3 Cu3 K3 N9 O25.75'
_chemical_formula_weight         2461.19
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           60
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.8803(9)
_cell_length_b                   28.4809(8)
_cell_length_c                   54.2721(16)
_cell_measurement_temperature    100(2)
_cell_volume                     38458(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.2801
_diffrn_reflns_av_sigmaI/netI    0.0727
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       63
_diffrn_reflns_limit_l_min       -64
_diffrn_reflns_number            424187
_diffrn_reflns_theta_full        66.50
_diffrn_reflns_theta_max         66.50
_diffrn_reflns_theta_min         2.36
_exptl_absorpt_coefficient_mu    1.726
_exptl_absorpt_correction_T_max  0.9436
_exptl_absorpt_correction_T_min  0.6683
_exptl_crystal_density_diffrn    0.850
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             10340
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.072
_refine_diff_density_min         -1.038
_refine_diff_density_rms         0.217
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.321
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1422
_refine_ls_number_reflns         33780
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.321
_refine_ls_R_factor_all          0.3381
_refine_ls_R_factor_gt           0.2159
_refine_ls_shift/su_max          5.804
_refine_ls_shift/su_mean         0.159
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4590
_refine_ls_wR_factor_ref         0.5138
_reflns_number_gt                13378
_reflns_number_total             33780
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic502873d_si_001.cif
_cod_data_source_block           gian2
_cod_depositor_comments
'Adding full bibliography for 4342504--4342510.cif.'
_cod_original_formula_sum        'C113 H150.50 Cl3 Cu3 K3 N9 O25.75'
_cod_database_code               4342507