Characterization of 3-D Metal−Organic Frameworks Formed through Hydrogen Bonding Interactions of 2-D Networks with Rectangular Voids by CoII- and NiII-Pyridine-2,6-dicarboxylate and 4,4‘-Bipyridine or 1,2-Di(pyridyl)ethylene
Ghosh, Sujit K.; Ribas, Joan; Bharadwaj, Parimal K.; Crystal Growth & Design 5 (2005) 623–; doi:10.1021/cg049838e

data_4505044
_publ_section_title
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 Characterization of 3-D Metal&#x2212;Organic Frameworks Formed through
 Hydrogen Bonding Interactions of 2-D Networks with Rectangular Voids by
 CoII- and NiII-Pyridine-2,6-dicarboxylate and 4,4&#x2018;-Bipyridine or
 1,2-Di(pyridyl)ethylene
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_journal_issue                   2
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              623
_journal_paper_doi               10.1021/cg049838e
_journal_volume                  5
_journal_year                    2005
_chemical_formula_moiety         'C26 H28 N4 Ni O13'
_chemical_formula_sum            'C26 H28 N4 Ni O13'
_chemical_formula_weight         663.23
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000
_cell_angle_beta                 96.083(5)
_cell_angle_gamma                90.000
_cell_formula_units_Z            4
_cell_length_a                   8.915(2)
_cell_length_b                   19.844(6)
_cell_length_c                   15.799(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      18
_cell_volume                     2779.3(14)
_computing_cell_refinement       CAD4
_computing_data_collection       'CAD4 Mach2'
_computing_data_reduction        SHELXL-97
_computing_molecular_graphics    'Diamond 2.1e'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.002
_diffrn_measurement_device_type  'Enraf-Nonius CAD4 Mach2'
_diffrn_measurement_method       'theta-2theta scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0213
_diffrn_reflns_av_sigmaI/netI    0.0258
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            3912
_diffrn_reflns_theta_full        22.48
_diffrn_reflns_theta_max         22.48
_diffrn_reflns_theta_min         1.65
_diffrn_standards_decay_%        <0.5
_diffrn_standards_interval_time  '1 h'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.775
_exptl_absorpt_correction_T_max  0.9196
_exptl_absorpt_correction_T_min  0.8795
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SHELXL routine in SHELX-97'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.585
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Rectangular parallelopiped'
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.355
_refine_diff_density_min         -0.628
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         3639
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0692P)^2^+1.5019P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0999
_refine_ls_wR_factor_ref         0.1169
_reflns_number_gt                2873
_reflns_number_total             3639
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg049838esi20040809_034529.cif
_cod_data_source_block           (dpeH2)[Ni(pdc)2].5H2O,_3.
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        2779.2(19)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4505044