Metallatubulane: synthesis and structural analysis of an infinite tubular coordination network formed by the self-assembly of a tetracyanocyclophane and silver cations
Kleina, Cédric; Graf, Ernest; Hosseini, Mir Wais; De Cian, André; Fischer, Jean; Chemical Communications  (2000) 239–; doi:10.1039/a909029k

data_7110791
_publ_section_title
;
 Metallatubulane: synthesis and structural analysis of an infinite tubular
 coordination network formed by the self-assembly of a
 tetracyanocyclophane and silver cations
;
_journal_issue                   3
_journal_name_full               'Chemical Communications'
_journal_page_first              239
_journal_paper_doi               10.1039/a909029k
_journal_year                    2000
_chemical_formula_moiety         C22H22N2AgPF6.MeOH.0.75CH2Cl2
_chemical_formula_sum            'C95 H110 Ag4 Cl6 F24 N8 O4 P4'
_chemical_formula_weight         2652.04
_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'
_cell_angle_alpha                90
_cell_angle_beta                 108.051(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   24.2853(5)
_cell_length_b                   19.1082(7)
_cell_length_c                   11.9631(4)
_cell_measurement_reflns_used    28326
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.4
_cell_volume                     5278.2(3)
_computing_publication_material  CIFGEN_IN_OpenMoleN_(_1997)
_computing_structure_refinement  LSFM_OpenMoleN_(_1997)
_computing_structure_solution    Direct_methods_(SIR,_Burla_et_al.,_1989)
_diffrn_ambient_temperature      173
_diffrn_measurement_details
;
  28326 reflections were collected using program Collect
 ("Collect" Data collection software, Nonius B.V., 1998)
 The conditions were as follow : crystal to detector distance =  36. mm.
 Scan angle =  2.0 deg 1 scans of  150 sec per frame.
 Data collection was divided into  4 set(s)
 with the following starting angles and number of frames :

 Set 1 Theta =    8.40 Omega = -216.00 Kappa =  180.00   86 frames
 Set 2 Theta =   -8.00 Kappa =   48.40 Phi   =   95.00   31 frames
 Set 3 Theta =   -6.20 Kappa =  193.00 Phi   = -203.00   48 frames
 Set 4 Theta =   -8.20 Kappa =  -29.00 Phi   =  105.00   29 frames
 Friedel pairs were averaged. Internal R = 0.04
;
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\p scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.040
_diffrn_reflns_av_sigmaI/netI    0.333
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            28326
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         2.5
_diffrn_source                   xray_tube
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.039
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.67
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             2668
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.983
_refine_diff_density_min         -0.673
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   2.527
_refine_ls_goodness_of_fit_ref   1.521
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     340
_refine_ls_number_reflns         3937
_refine_ls_number_restraints     38
_refine_ls_R_factor_all          0.097
_refine_ls_R_factor_gt           0.063
_refine_ls_shift/esd_mean        0.001
_refine_ls_shift/su_max          0.045
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 4Fo^2^/(\s^2^(Fo^2^)+0.0004 Fo^4^)+2.0'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.141
_refine_ls_wR_factor_ref         0.083
_reflns_number_gt                3937
_reflns_number_total             6246
_reflns_threshold_expression     >3.0\s(I)
_cod_data_source_file            a909029ksup1.cif
_cod_data_source_block           st472
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '4Fo^2^/(\s^2^(Fo^2^)+0.0004
Fo^4^)+2.0' was changed to 'calc'. New tag
'_refine_ls_weighting_details' was created. The value of the new tag
was set to 'w = 4Fo^2^/(\s^2^(Fo^2^)+0.0004 Fo^4^)+2.0'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        5278.2(5)
_cod_database_code               7110791