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_1513026
_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 H24 Mn N4 O5'
_chemical_formula_sum            'C24 H24 Mn N4 O5'
_chemical_formula_weight         503.41
_chemical_name_systematic
;
catena-((\m~3~-Biphenyl-2,2'-dicarboxylato)-(3,3',5,5'-tetramethyl-
4,4'-bipyrazole)-aqua-manganese(ii))
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 95.224(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.5422(4)
_cell_length_b                   10.4750(4)
_cell_length_c                   22.8707(9)
_cell_measurement_reflns_used    20722
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      29.165
_cell_measurement_theta_min      3.30
_cell_volume                     2276.54(16)
_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 8.192
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0249
_diffrn_reflns_av_sigmaI/netI    0.0300
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5490
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         3.30
_exptl_absorpt_coefficient_mu    0.624
_exptl_absorpt_correction_T_max  0.8972
_exptl_absorpt_correction_T_min  0.8354
_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    1.469
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1044
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.393
_refine_diff_density_min         -0.245
_refine_diff_density_rms         0.048
_refine_ls_extinction_coef       0.0018(4)
_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   0.940
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         5490
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.940
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0243
_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^)+(0.0390P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0585
_refine_ls_wR_factor_ref         0.0598
_reflns_number_gt                4368
_reflns_number_total             5490
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-397-60-68-1.cif
_cod_data_source_block           1
_cod_original_cell_volume        2276.53(16)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1513026