Hydrothermal Synthesis and Structure of Coordination Polymers by Combination of Bipyrazole and Aromatic Dicarboxylate Ligands
Hunger, Jens; Krautscheid, Harald; Sieler, Joachim; Crystal Growth & Design 9 (2009) 4613–; doi:10.1021/cg801282r

data_4509360
_publ_section_title
;
 Hydrothermal Synthesis and Structure of Coordination Polymers by
 Combination of Bipyrazole and Aromatic Dicarboxylate Ligands
;
_journal_issue                   11
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              4613
_journal_paper_doi               10.1021/cg801282r
_journal_volume                  9
_journal_year                    2009
_chemical_formula_moiety         '2(C36 H36 N8 O10 Zn2), H2 O, 2.20(O)'
_chemical_formula_sum            'C72 H74 N16 O23.2 Zn4'
_chemical_formula_weight         1796.30
_chemical_name_systematic
;
catena-(bis(\m~2~-5-hydroxy-benzene-1,3-dicarboxylato)-bis(\m~2~-3,3',5,5'-
tetramethyl-4,4'-bipyrazole)-di-zinc(ii) hydrate)
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 100.549(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.9736(15)
_cell_length_b                   21.3073(16)
_cell_length_c                   27.066(3)
_cell_measurement_reflns_used    7911
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      26.9
_cell_measurement_theta_min      7.4
_cell_volume                     7922.4(14)
_computing_cell_refinement       'RECIPE (Stoe & Cie, 2002)'
_computing_data_collection       'EXPOSE (Stoe & Cie, 2002)'
_computing_data_reduction        'INTEGRATE (Stoe & Cie, 2002)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXL97 and DIAMOND'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Stoe IPDS-I'
_diffrn_measurement_method       \w
_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  0.0431
_diffrn_reflns_av_sigmaI/netI    0.0331
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            43422
_diffrn_reflns_theta_full        26.91
_diffrn_reflns_theta_max         26.91
_diffrn_reflns_theta_min         2.51
_exptl_absorpt_coefficient_mu    1.282
_exptl_absorpt_correction_T_max  0.7146
_exptl_absorpt_correction_T_min  0.5276
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
[X-RED32 (Stoe & Cie, 2001);
crystal description using FACEIT (Stoe & Cie, 2002);
optimization using equivalent reflections
(X-SHAPE; Stoe & Cie, 1999)]
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3694.4
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.518
_refine_diff_density_min         -0.288
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.882
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     602
_refine_ls_number_reflns         8499
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      0.887
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0279
_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^)+(0.0462P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0668
_refine_ls_wR_factor_ref         0.0683
_reflns_number_gt                6449
_reflns_number_total             8499
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg801282rsup1.cif
_cod_data_source_block           8
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C72 H74 N16 O23.20 Zn4'
_cod_database_code               4509360