1,2,4,5-Benzenetetrasulfonic acid and 1,4-benzenedisulfonic acid as sulfo analogues of pyromellitic and terephthalic acids for building coordination polymers of manganese
Zitzer, Christina; Muesmann, Thomas W. T.; Christoffers, Jens; Schwickert, Christian; Pöttgen, Rainer; Wickleder, Mathias S.; CrystEngComm 16 (2014) 11064–; doi:10.1039/C4CE01618A

data_7218508
_publ_section_title
;
 1,2,4,5-Benzenetetrasulfonic acid and 1,4-benzenedisulfonic acid as sulfo
 analogues of pyromellitic and terephthalic acids for building
 coordination polymers of manganese
;
_journal_issue                   48
_journal_name_full               CrystEngComm
_journal_page_first              11064
_journal_paper_doi               10.1039/C4CE01618A
_journal_volume                  16
_journal_year                    2014
_chemical_formula_sum            'C26 H40 Mn N4 O16 S4'
_chemical_formula_weight         847.80
_chemical_name_common
(hydroxymethyldihydropyrrolium)(manganese(II)-(benezenetetrasulfonate))(N-methylpyrrolidone)
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 113.529(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.3170(7)
_cell_length_b                   10.4919(7)
_cell_length_c                   19.4487(12)
_cell_measurement_temperature    120(2)
_cell_volume                     1743.1(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120.15
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.962
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0512
_diffrn_reflns_av_unetI/netI     0.0384
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            77638
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.875
_diffrn_reflns_theta_min         2.252
_exptl_absorpt_coefficient_mu    0.697
_exptl_absorpt_correction_T_max  0.935
_exptl_absorpt_correction_T_min  0.863
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.615
_exptl_crystal_description       needles
_exptl_crystal_F_000             882
_exptl_crystal_size_max          0.218
_exptl_crystal_size_mid          0.135
_exptl_crystal_size_min          0.098
_refine_diff_density_max         1.104
_refine_diff_density_min         -0.465
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         5757
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0818
_refine_ls_R_factor_gt           0.0501
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0781P)^2^+0.9186P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1310
_refine_ls_wR_factor_ref         0.1484
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4016
_reflns_number_total             5757
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4ce01618a1.cif
_cod_data_source_block           c:\cz211a\cz211a
_cod_depositor_comments
'Adding full bibliography for 7218507--7218511.cif.'
_cod_database_code               7218508
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O2-H2
 0.85 with sigma of 0.001
 C22A-C23A
 1.5 with sigma of 0.001
3. Others
 Fixed Sof: O11(0.6) O12(0.6) O13(0.6) O14(0.6) O15(0.6) O16(0.6) O11A(0.4)
 O12A(0.4) O13A(0.4) O14A(0.4) O15A(0.4) O16A(0.4) O2(0.7) H2(0.7) C21(0.7)
 C22(0.7) H22a(0.7) H22b(0.7) C23(0.7) H23a(0.7) H23b(0.7) C24(0.7) H24a(0.7)
 H24b(0.7) N2(0.7) C25(0.7) H25a(0.7) H25b(0.7) H25c(0.7) O2A(0.3) C21A(0.3)
 C22A(0.3) C23A(0.3) C24A(0.3) N2A(0.3) C25A(0.3)
4.a Secondary CH2 refined with riding coordinates:
 C12(H12a,H12b), C13(H13a,H13b), C14(H14a,H14b), C22(H22a,H22b), C23(H23a,
 H23b), C24(H24a,H24b)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3)
4.c Idealised Me refined as rotating group:
 C15(H15a,H15b,H15c), C25(H25a,H25b,H25c)
;
_shelx_res_checksum              2659
_olex2_submission_special_instructions 'No special instructions were received'