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_1513028
_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         'C30 H42 Ag2 N12, 2(C2 H3 O2), 1.56(H2 O) '
_chemical_formula_sum            'C34 H51.12 Ag2 N12 O5.56'
_chemical_formula_weight         932.71
_chemical_name_systematic
;
catena-(Diaqua-tris(\m~2~-3,3',5,5'-tetramethyl-
4,4'-bipyrazole)-disilver(i)) diacetate
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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            8
_cell_length_a                   17.8084(6)
_cell_length_b                   18.8997(6)
_cell_length_c                   24.4847(7)
_cell_measurement_reflns_used    41135
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      29.20
_cell_measurement_theta_min      3.25
_cell_volume                     8240.9(4)
_computing_cell_refinement       'RECIPE (Stoe & Cie, 2002)'
_computing_data_collection       'WinXpose (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      100(1)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Stoe IPDS-2T'
_diffrn_measurement_method       '\w-scan and \f-scan'
_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  0.0415
_diffrn_reflns_av_sigmaI/netI    0.0165
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            35173
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.01
_diffrn_reflns_theta_min         3.25
_exptl_absorpt_coefficient_mu    1.006
_exptl_absorpt_correction_T_max  0.7677
_exptl_absorpt_correction_T_min  0.6101
_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    1.503
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3821
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.33
_refine_diff_density_max         0.738
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       0.00022(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     518
_refine_ls_number_reflns         9921
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0249
_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^)+(0.0179P)^2^+2.1059P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0665
_refine_ls_wR_factor_ref         0.0694
_reflns_number_gt                7833
_reflns_number_total             9921
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-397-60-68-3.cif
_cod_data_source_block           3
_cod_database_code               1513028