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_7207400
_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         'C31 H35 Cd N7 O7'
_chemical_formula_sum            'C31 H35 Cd N7 O7'
_chemical_formula_weight         730.06
_chemical_name_systematic
;
?
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 100.5740(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.1191(5)
_cell_length_b                   18.8297(11)
_cell_length_c                   18.7331(12)
_cell_measurement_reflns_used    5550
_cell_measurement_temperature    185(2)
_cell_measurement_theta_max      26.09
_cell_measurement_theta_min      1.55
_cell_volume                     2815.3(3)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0417
_diffrn_reflns_av_sigmaI/netI    0.0510
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            15363
_diffrn_reflns_theta_full        26.09
_diffrn_reflns_theta_max         26.09
_diffrn_reflns_theta_min         1.55
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    0.842
_exptl_absorpt_correction_T_max  0.8985
_exptl_absorpt_correction_T_min  0.8365
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.722
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_platon_squeeze_details
;
Attempts to refine peaks of residual electron density
as guest atoms were unsuccessful,
although the atoms of the (DMF) solvent
molecule were observed but could not be modeled
satisfactorily during the structure
refinement. The data were corrected for disordered
electron density through use of the
SQUEEZE procedure (Sluis, P. van der;
Spek, A. L. Acta Crystallogr. 1990,
A46, 194-201) as implemented in PLATON
(Spek, A.L. Acta Crystallogr. 1990, A46, C34.
PLATON C a multipurpose crystallographic tool.
Utrecht University, Utrecht, The Netherlands).
A total solvent-accessible
void volume of 1062.0 A^3^ with a total electron count of 600
(consistent with ca. three molecules of
solvent DMF per formula
characterized by elemental and
thermo-gravimetric analysis) was found in the unit cell.
;
_refine_diff_density_max         0.601
_refine_diff_density_min         -1.268
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         5550
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0373
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0552P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1009
_refine_ls_wR_factor_ref         0.1048
_reflns_number_gt                4119
_reflns_number_total             5550
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce05948g.txt
_cod_data_source_block           m2
_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_sg_symbol_H-M      P21/c
_cod_database_code               7207400