Hydroxyl- and chloro-bridges as “structural assistants” in the construction of two new Keggin-based 3D frameworks
Tian, AiXiang; Lin, XiaoLing; Liu, XiaoJing; Ying, Jun; Wang, XiuLi; RSC Advances 3 (2013) 17188–; doi:10.1039/c3ra41567h

data_7239058
_publ_section_title
;
 Hydroxyl- and chloro-bridges as &#x201C;structural assistants&#x201D; in
 the construction of two new Keggin-based 3D frameworks
;
_journal_issue                   38
_journal_name_full               'RSC Advances'
_journal_page_first              17188
_journal_paper_doi               10.1039/c3ra41567h
_journal_volume                  3
_journal_year                    2013
_chemical_formula_sum            'C16 H25 Cu4 N12 O41 P W12'
_chemical_formula_weight         3533
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/m 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                 98.752(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.774(5)
_cell_length_b                   19.299(5)
_cell_length_c                   11.056(5)
_cell_measurement_temperature    293(2)
_cell_volume                     2693.8(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_sigmaI/netI    0.0432
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11670
_diffrn_reflns_theta_full        26.07
_diffrn_reflns_theta_max         26.07
_diffrn_reflns_theta_min         2.50
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    27.180
_exptl_absorpt_correction_T_max  0.013
_exptl_absorpt_correction_T_min  0.005
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'ABSCOR by T.Higashi    8  March, 1995'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    4.354
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3102
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_refine_diff_density_max         2.338
_refine_diff_density_min         -3.512
_refine_diff_density_rms         0.311
_refine_ls_extinction_coef       0.00043(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   0.985
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         2758
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0378
_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^)+(0.0621P)^2^+92.0419P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1048
_refine_ls_wR_factor_ref         0.1108
_reflns_number_gt                2340
_reflns_number_total             2765
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ra41567h.txt
_cod_data_source_block           compound-1
_cod_original_sg_symbol_H-M      C2/m
_cod_database_code               7239058