Three unprecedented open frameworks based on a pyridyl-carboxylate: synthesis, structures and properties
Su, Shengqun; Chen, Wan; Song, Xuezhi; Zhu, Min; Qin, Chao; Song, Shuyan; Guo, Zhiyong; Wang, Song; Hao, Zhaoming; Li, Guanghua; Zhang, Hongjie; CrystEngComm 14 (2012) 1681–; doi:10.1039/c2ce05948g

data_7207398
_publ_section_title
;
 Three unprecedented open frameworks based on a pyridyl-carboxylate:
 synthesis, structures and properties
;
_journal_issue                   5
_journal_name_full               CrystEngComm
_journal_page_first              1681
_journal_paper_doi               10.1039/c2ce05948g
_journal_volume                  14
_journal_year                    2012
_chemical_formula_moiety         'C25 H21 N5 Ni O5'
_chemical_formula_sum            'C25.9 H23.1 N5.3 Ni O5.3'
_chemical_formula_weight         552.11
_chemical_melting_point          ?
_chemical_name_systematic
;
?
;
_space_group_IT_number           90
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4ab 2ab'
_symmetry_space_group_name_H-M   'P 4 21 2'
_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                   22.3163(5)
_cell_length_b                   22.3163(5)
_cell_length_c                   12.7222(6)
_cell_measurement_reflns_used    6259
_cell_measurement_temperature    185(2)
_cell_measurement_theta_max      26.02
_cell_measurement_theta_min      1.60
_cell_volume                     6335.9(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    SHELXP-97
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      185(2)
_diffrn_detector_area_resol_mean 9.00cm
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0598
_diffrn_reflns_av_sigmaI/netI    0.0419
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            35274
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         1.60
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    0.651
_exptl_absorpt_correction_T_max  0.8753
_exptl_absorpt_correction_T_min  0.7899
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.158
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2288
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_platon_squeeze_details
;
During the structure refinement, the atoms of the (DMF) solvent molecule were observed but could not be modeled satisfactorily. Therefore, the SQUEEZE routine in PLATON was used to modify the HKL file and the solvent equated to 1.3 DMF molecules per formula.
;
_refine_diff_density_max         0.599
_refine_diff_density_min         -0.731
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.52(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         6259
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0470
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0728P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1174
_refine_ls_wR_factor_ref         0.1225
_reflns_number_gt                4912
_reflns_number_total             6259
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce05948g.txt
_cod_data_source_block           tb
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_symmetry_cell_setting' value
'Tetragonal' changed to 'tetragonal' 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 

The following automatic conversions were performed:

'_refine_ls_hydrogen_treatment' value 'constra' was replaced with the
value 'constr' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_original_sg_symbol_H-M      P42(1)2
_cod_original_formula_sum        'C25.90 H23.10 N5.30 Ni O5.30'
_cod_database_code               7207398