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_4342509
_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            'C123.55 H174.6 N11 Na Ni2 O20.5'
_chemical_formula_weight         2282.35
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2014-07-14 # Formatted by publCIF

;
_cell_angle_alpha                90.00
_cell_angle_beta                 96.148(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.1740(9)
_cell_length_b                   25.4074(14)
_cell_length_c                   29.3905(16)
_cell_measurement_reflns_used    9891
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.01
_cell_measurement_theta_min      2.24
_cell_volume                     12750.7(12)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2 (Bruker, 2008)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL (Bruker, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II DUO'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Bruker Triumph'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0660
_diffrn_reflns_av_sigmaI/netI    0.0697
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            180391
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.06
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.366
_exptl_absorpt_correction_T_max  0.9478
_exptl_absorpt_correction_T_min  0.8863
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             4896
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.711
_refine_diff_density_min         -1.057
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.457
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1337
_refine_ls_number_reflns         29303
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.459
_refine_ls_R_factor_all          0.1339
_refine_ls_R_factor_gt           0.0821
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc 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          0.2319
_refine_ls_wR_factor_ref         0.2504
_reflns_number_gt                17628
_reflns_number_total             29303
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic502873d_si_005.cif
_cod_data_source_block           jess8
_cod_depositor_comments
'Adding full bibliography for 4342504--4342510.cif.'
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C123.55 H174.60 N11 Na Ni2 O20.50'
_cod_database_code               4342509