Synthesis and structure of coordination polymers of Mn2+, Cu2+, Ag+, Zn2+ and Cd2+ by combination of bipyrazole and diphenate ligands
Jens Hunger; Inorganica Chimica Acta 397 (2013) 60–68; doi:10.1016/j.ica.2012.11.019

data_1513029
_publ_section_title
;
 Synthesis and structure of coordination polymers of Mn2+, Cu2+, Ag+, Zn2+
 and Cd2+ by combination of bipyrazole and diphenate ligands
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              60
_journal_page_last               68
_journal_paper_doi               10.1016/j.ica.2012.11.019
_journal_volume                  397
_journal_year                    2013
_chemical_formula_moiety         'C24 H22 N4 O4 Zn, 0.61(H2 O)'
_chemical_formula_sum            'C24 H23.21 N4 O4.61 Zn'
_chemical_formula_weight         506.75
_chemical_name_systematic
;
catena-((\m~2~-Biphenyl-2,2'-dicarboxylato)-(\m~2~-3,3',5,5'-tetramethyl-
4,4'-bipyrazole)-zinc(ii) hemihydrate)
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.1779(9)
_cell_length_b                   13.3676(14)
_cell_length_c                   16.3999(18)
_cell_measurement_reflns_used    33635
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      28.00
_cell_measurement_theta_min      2.50
_cell_volume                     2450.5(4)
_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 0.982
_diffrn_measured_fraction_theta_max 0.961
_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  0.0377
_diffrn_reflns_av_sigmaI/netI    0.0703
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            33635
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.48
_exptl_absorpt_coefficient_mu    1.041
_exptl_absorpt_correction_T_max  0.7683
_exptl_absorpt_correction_T_min  0.6642
_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            colourless
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.59
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.358
_refine_diff_density_min         -0.233
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.005(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.903
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         5722
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      0.905
_refine_ls_R_factor_all          0.0330
_refine_ls_R_factor_gt           0.0243
_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^)+(0.0559P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0419
_refine_ls_wR_factor_ref         0.0425
_reflns_number_gt                4216
_reflns_number_total             5722
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-397-60-68-4.cif
_cod_data_source_block           4
_cod_database_code               1513029