Crystal Structure Solid-State Cross Polarization Magic Angle Spinning 13C NMR Correlation in Luminescent d10 Metal-Organic Frameworks Constructed with the 1,2-Bis(1,2,4-triazol-4-yl)ethane Ligand
Hesham A. Habib; Anke Hoffmann; Henning A. Höppe; Gunther Steinfeld; Christoph Janiak; Inorganic Chemistry 48 (2009) 2166–2180; doi:10.1021/ic802069k

data_4301604
_publ_contact_author_address
;Institut f\"ur Anorganische und Analytische Chemie
Universit\"at Freiburg
Albertstr. 21
79104 Freiburg
Germany
;
_publ_contact_author_email       janiak@uni-freiburg.de
_publ_contact_author_name        'Christoph Janiak'
_publ_contact_author_phone       +49-761-2036127
_publ_section_title
;
Crystal Structure Solid-State Cross Polarization Magic Angle Spinning 13C
NMR Correlation in Luminescent d10 Metal-Organic Frameworks Constructed with
the 1,2-Bis(1,2,4-triazol-4-yl)ethane Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2166
_journal_page_last               2180
_journal_paper_doi               10.1021/ic802069k
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C9 H16 Cd3 N9 O17 S2.5'
_chemical_formula_weight         939.66
_chemical_name_systematic
; 
catena-{triaqua-1.5{\m4-1,2-bis(1,2,4-triazol-4-yl)ethane-
\kN1:\kN2:\kN1':\kN2'}-\m3-hydroxo-bis{\m3-sulfato-\kO:\kO':\kO''}-
tricadmium-semi-sulfate-trihydrate} 
;
_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                 101.5040(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   28.0573(7)
_cell_length_b                   9.0053(2)
_cell_length_c                   21.2997(5)
_cell_measurement_reflns_used    9936
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      38.37
_cell_measurement_theta_min      2.50
_cell_volume                     5273.6(2)
_computing_cell_refinement       'SAINT (Bruker, 2006)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'DIAMOND (Crystal Impact, 2006)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX II CCD area detector'
_diffrn_measurement_method       '\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  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0246
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            27302
_diffrn_reflns_theta_full        26.90
_diffrn_reflns_theta_max         26.90
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    2.687
_exptl_absorpt_correction_T_max  0.8774
_exptl_absorpt_correction_T_min  0.3843
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.367
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             3624
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.162
_refine_diff_density_min         -0.735
_refine_diff_density_rms         0.171
_refine_ls_extinction_coef       0.00242(7)
_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   1.360
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     405
_refine_ls_number_reflns         5648
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.360
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0433
_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^)+(0.0000P)^2^+115.7791P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1030
_refine_ls_wR_factor_ref         0.1033
_reflns_number_gt                5531
_reflns_number_total             5648
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic802069k_si_002_07.cif
_cod_data_source_block           m196_2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-scan' changed
to 'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C9 H16 Cd3 N9 O17 S2.50'
_cod_database_code               4301604