Natural abundance 13C and 15N solid-state NMR analysis of paramagnetic transition-metal cyanide coordination polymers
Aguiar, Pedro M.; Katz, Michael J.; Leznoff, Daniel B.; Kroeker, Scott; Physical Chemistry Chemical Physics 11 (2009) 6925–6934; doi:10.1039/b907747b

data_7201300
_publ_section_title
;
 Natural abundance 13C and 15N solid-state NMR analysis of paramagnetic
 transition-metal cyanide coordination polymers
;
_journal_issue                   32
_journal_name_full               'Physical Chemistry Chemical Physics'
_journal_page_first              6925
_journal_page_last               6934
_journal_paper_doi               10.1039/b907747b
_journal_volume                  11
_journal_year                    2009
_chemical_formula_moiety         'C8 H16 Au2 N8 Zn1'
_chemical_formula_sum            'C8 H16 Au2 N8 Zn'
_chemical_formula_weight         683.59
_chemical_name_systematic        ?
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 119.508(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.516(3)
_cell_length_b                   13.2522(19)
_cell_length_c                   6.4403(11)
_cell_measurement_reflns_used    618
_cell_measurement_temperature    293.1500
_cell_measurement_theta_max      71.5862
_cell_measurement_theta_min      5.8756
_cell_volume                     781.1(3)
_computing_cell_refinement
; 
'CrystalClear (Rigaku/MSC Inc., 2005)'
;
_computing_data_collection
; 
'CrystalClear (Rigaku/MSC Inc., 2005)'
;
_computing_data_reduction
; 
'CrystalClear (Rigaku/MSC Inc., 2005)'
;
_computing_structure_refinement
;
CRYSTALS (Betteridge et al., 2003) 
;
_computing_structure_solution
; 
SIR92 (Altomare et al, 1994) 
;
_diffrn_ambient_temperature      293.1500
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_details
;
scan:
    Number of images: 17
               Slice: 0.0000 - 170.0000
         Image width: 10.0000
            Exp time: 600.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 0.0000
                 Phi: 0.0000
                 XTD: 127.4000
              2theta: -0.0012
scan:
    Number of images: 17
               Slice: 0.0000 - 170.0000
         Image width: 10.0000
            Exp time: 600.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 127.4000
              2theta: -0.0012
scan:
    Number of images: 14
               Slice: 0.0000 - 144.0000
         Image width: 10.0000
            Exp time: 600.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 180.0000
                 XTD: 127.4000
              2theta: -0.0012
scan:
    Number of images: 8
               Slice: 0.0000 - 80.0000
         Image width: 10.0000
            Exp time: 600.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 0.0000
                 Phi: 90.0000
                 XTD: 127.4000
              2theta: -0.0012
scan:
    Number of images: 6
               Slice: 65.0000 - 130.0000
         Image width: 10.0000
            Exp time: 600.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 36.0000
                 Phi: 90.0000
                 XTD: 127.4000
              2theta: -0.0012
scan:
    Number of images: 18
               Slice: 0.0000 - 184.0000
         Image width: 10.0000
            Exp time: 600.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 90.0000
                 XTD: 127.4000
              2theta: -0.0012

;
_diffrn_measurement_device_details
;
Crystal Goniometer
;
_diffrn_measurement_device_type
;
RAXIS conversion
;
_diffrn_measurement_method       dtprofit.ref
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.0892
_diffrn_orient_matrix_UB_12      -0.0591
_diffrn_orient_matrix_UB_13      0.0223
_diffrn_orient_matrix_UB_21      -0.0222
_diffrn_orient_matrix_UB_22      0.0063
_diffrn_orient_matrix_UB_23      -0.0719
_diffrn_orient_matrix_UB_31      0.0056
_diffrn_orient_matrix_UB_32      -0.1775
_diffrn_orient_matrix_UB_33      -0.0173
_diffrn_radiation_detector       RX
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_source         'Sealed Tube'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.105
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            4033
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        42.391
_diffrn_reflns_theta_max         71.849
_diffrn_reflns_theta_min         5.876
_diffrn_source_current           42.0000
_diffrn_source_power             1.9320
_diffrn_source_voltage           46.0000
_exptl_absorpt_coefficient_mu    36.412
_exptl_absorpt_correction_T_max  0.4010
_exptl_absorpt_correction_T_min  0.0635
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.906
_exptl_crystal_description       'needle '
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.70
_refine_diff_density_min         -2.80
_refine_ls_extinction_coef       27(2)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.0244
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     56
_refine_ls_number_reflns         590
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0432
_refine_ls_shift/su_max          0.000027
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method= Modified Sheldrick 
w=1/[\s^2^(F^2^) + ( 0.01P)^2^ + 0.00P] 
,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1232
_refine_ls_wR_factor_gt          0.0652
_refine_ls_wR_factor_ref         0.0594
_reflns_limit_h_max              11
_reflns_limit_h_min              -12
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              7
_reflns_limit_l_min              0
_reflns_number_gt                649
_reflns_number_total             751
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.88
_oxford_diffrn_Wilson_scale      1.31
_oxford_refine_ls_r_factor_ref   0.0410
_oxford_refine_ls_scale          1.170(13)
_oxford_reflns_number_all        747
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            b907747b.cif
_cod_data_source_block           Zn(en)2[Au(CN)2]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 'Numerical' changed to
'numerical' 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 1 2/m 1 '
_cod_original_formula_sum        'C8 H16 Au2 N8 Zn1'
_cod_database_code               7201300
_diffrn_number_total             751
_diffrn_reflns_av_sigmai/deti    0.1266