Poly[tetraaqua-μ~4~-bromido-di-μ~2~-bromido-μ~2~-hydroxido-di-μ~3~-isonicotinato-tetra-μ~2~-isonicotinato-tetracopper(I)dithulium(III)]
Wang, Guo-Ming; Li, Zeng-Xin; Zheng, Qing-Hua; Liu, Hui-Luan; Acta Crystallographica Section E 64 (2008) m1260–m1261; doi:10.1107/S1600536808028675

data_2219716
_publ_section_title
Poly[tetraaqua-\m~4~-bromido-di-\m~2~-bromido-\m~2~-hydroxido-di-\m~3~-isonicotinato-tetra-\m~2~-isonicotinato-tetracopper(I)dithulium(III)]
_journal_coeditor_code           SJ2536
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1260
_journal_page_last               m1261
_journal_paper_doi               10.1107/S1600536808028675
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Cu4 Tm2 Br3 (C6 H4 N O2)6 (O H) (H2 O)4]'
_chemical_formula_moiety         'C36 H33 Br3 Cu4 N6 O17 Tm2'
_chemical_formula_sum            'C36 H33 Br3 Cu4 N6 O17 Tm2'
_chemical_formula_weight         1653.43
_chemical_name_systematic
;
Poly[tetraaqua-\m~4~-bromido-di-\m~2~-bromido-\m~2~-hydroxido-di-\m~3~-
isonicotinato-tetra-\m~2~-isonicotinato-tetracopper(I)dithulium(III)]
;
_space_group_IT_number           63
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.1815(2)
_cell_length_b                   6.6973(4)
_cell_length_c                   34.7044(5)
_cell_measurement_reflns_used    6070
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      26.49
_cell_measurement_theta_min      2.12
_cell_volume                     4458.3(3)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'APEX2 (Bruker, 2002)'
_computing_data_reduction        'SAINT (Bruker, 2002)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEXII area-detector'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0369
_diffrn_reflns_av_sigmaI/netI    0.0233
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            17231
_diffrn_reflns_theta_full        26.49
_diffrn_reflns_theta_max         26.49
_diffrn_reflns_theta_min         2.12
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.580
_exptl_absorpt_correction_T_max  0.5469
_exptl_absorpt_correction_T_min  0.3406
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.463
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3144
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.829
_refine_diff_density_min         -0.873
_refine_ls_extinction_coef       0.00119(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         2408
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_gt           0.0268
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0288P)^2^+11.1134P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0612
_refine_ls_wR_factor_ref         0.0641
_reflns_number_gt                2090
_reflns_number_total             2408
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sj2536.cif
_cod_data_source_block           I
_cod_database_code               2219716
_cod_database_fobs_code          2219716