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_4342504
_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
'C90 H99 N9 O16 Ni2, 2(C8 H20 N1), 5(C4 H8 O1), (C4 H10 O1), 0.2(H2O)'
_chemical_formula_sum            'C130 H191.4 N11 Ni2 O23.2'
_chemical_formula_weight         2396.96
_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
;
2014-04-07 # Formatted by publCIF

;
_cell_angle_alpha                90.00
_cell_angle_beta                 95.621(1)
_cell_angle_gamma                90.00
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_cell_length_a                   17.1944(8)
_cell_length_b                   25.4173(11)
_cell_length_c                   29.5150(13)
_cell_measurement_reflns_used    9625
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.0
_cell_volume                     12837.1(10)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2 (Bruker, 2008)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2008)'
_computing_molecular_graphics    'SHELXL-2013 (Sheldrick, 2013)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II DUO'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0681
_diffrn_reflns_av_sigmaI/netI    0.0550
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            177043
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.43
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.365
_exptl_absorpt_correction_T_max  0.9459
_exptl_absorpt_correction_T_min  0.8688
_exptl_absorpt_correction_type   analytical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_description       plates
_exptl_crystal_F_000             5160
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.668
_refine_diff_density_min         -0.887
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1513
_refine_ls_number_reflns         29441
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.1147
_refine_ls_R_factor_gt           0.0782
_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^)+(0.0695P)^2^+39.5228P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1796
_refine_ls_wR_factor_ref         0.1998
_reflns_number_gt                20850
_reflns_number_total             29441
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic502873d_si_007.cif
_cod_data_source_block           jess11
_cod_depositor_comments
'Adding full bibliography for 4342504--4342510.cif.'
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C130 H191.40 N11 Ni2 O23.20'
_cod_database_code               4342504