Solvothermal synthesis, multi-temperature crystal structures and physical properties of isostructural coordination polymers, 2C~4~H~12~N^+^[<i>M</i>~3~(C~8~H~4~O~4~)~4~]^2{-^}·3C~5~H~11~NO, <i>M</i> = Co, Zn
Damgaard Poulsen, Rasmus; Bentien, Anders; Christensen, Mogens; Brummerstedt Iversen, Bo; Acta Crystallographica Section B 62 (2006) 245–254; doi:10.1107/S0108768105042795

data_2100441
_publ_section_title
;
 Solvothermal synthesis, multi-temperature crystal structures and
 physical properties of isostructural coordination polymers,
 2C~4~H~12~N^+^[<i>M</i>~3~(C~8~H~4~O~4~)~4~]^2{-^}&#x00B7;3C~5~H~11~NO,
 <i>M</i> = Co, Zn
;
_journal_coeditor_code           LC5040
_journal_date_accepted           2005-12-22
_journal_date_recd_electronic    2005-09-21
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              245
_journal_page_last               254
_journal_paper_category          FA
_journal_paper_doi               10.1107/S0108768105042795
_journal_volume                  62
_journal_year                    2006
_chemical_formula_moiety         'C27.50 H36.50 N2.50 O9.50 Zn1.50'
_chemical_formula_sum            'C27.5 H36.5 N2.5 O9.5 Zn1.5'
_chemical_formula_weight         652.15
_chemical_name_systematic
;
 ?
;
_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                 92.5520(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   33.3307(5)
_cell_length_b                   9.81050(10)
_cell_length_c                   18.1988(3)
_cell_measurement_reflns_used    9872
_cell_measurement_temperature    100.0(10)
_cell_measurement_theta_max      27.73
_cell_measurement_theta_min      2.24
_cell_volume                     5944.94(15)
_computing_cell_refinement       'SMART (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100.0(10)
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  'Bruker SMART 1K CCD area-detector'
_diffrn_measurement_method       '\w and \p'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1131
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9010
_diffrn_reflns_theta_full        31.00
_diffrn_reflns_theta_max         31.00
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    1.277
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.863454
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1997)'
_exptl_crystal_colour            'white colourless'
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombic
_exptl_crystal_F_000             2720
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.250
_refine_diff_density_max         0.636
_refine_diff_density_min         -0.612
_refine_ls_extinction_coef       0.00052(9)
_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   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     430
_refine_ls_number_reflns         9010
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.1243
_refine_ls_R_factor_gt           0.0605
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0557P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1016
_refine_ls_wR_factor_ref         0.1173
_reflns_number_gt                5722
_reflns_number_total             9010
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            lc5040.cif
_cod_data_source_block           ZnBDCDEF_100K
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C27.50 H36.50 N2.50 O9.50 Zn1.50'
_cod_database_code               2100441