Multicomponent Self-Assembly: Generation of Rigid-Rack Multimetallic Pseudorotaxanes
Hanadi Sleiman; Paul N. W. Baxter; Jean-Marie Lehn; Karri Airola; Kari Rissanen; Inorganic Chemistry 36 (1997) 4734–4742; doi:10.1021/ic9702227

data_4323623
_publ_section_title
;
 Multicomponent Self-Assembly: Generation of Rigid-Rack Multimetallic
 Pseudorotaxanes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4734
_journal_page_last               4742
_journal_paper_doi               10.1021/ic9702227
_journal_volume                  36
_journal_year                    1997
_chemical_formula_structural     'C8 H7 N2 Cu+ C34 H34 N2 O6 PF6 -'
_chemical_formula_sum            'C42 H41 Cu F6 N4 O6 P'
_chemical_formula_weight         906.30
_chemical_name_common            '[3]-pseudorotaxane Cu complex'
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 95.18(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.199(4)
_cell_length_b                   17.227(3)
_cell_length_c                   21.109(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15.82
_cell_measurement_theta_min      9.28
_cell_volume                     8040(3)
_computing_cell_refinement       'Enraf-Nonius CAD4'
_computing_data_collection       'Enraf-Nonius CAD4'
_computing_data_reduction        'CADRED (Enraf-Nonius, 1988)'
_computing_molecular_graphics    'SCHAKAL 92 (Keller, 1992)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       two-theta/omega
_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  0.0517
_diffrn_reflns_av_sigmaI/netI    0.1241
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            5710
_diffrn_reflns_theta_max         22.98
_diffrn_reflns_theta_min         2.36
_diffrn_standards_decay_%        +-6
_diffrn_standards_interval_count '150 (orientation)'
_diffrn_standards_interval_time  '60 (intensity)'
_diffrn_standards_number         '2 (intensity), 3 (orientation)'
_exptl_absorpt_coefficient_mu    0.665
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.771
_exptl_absorpt_correction_type   'empirical with psi-scans'
_exptl_crystal_colour            red-violet
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prisms
_exptl_crystal_F_000             3736
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.597
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.014
_refine_ls_goodness_of_fit_obs   1.137
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     534
_refine_ls_number_reflns         5540
_refine_ls_number_restraints     87
_refine_ls_restrained_S_all      1.023
_refine_ls_restrained_S_obs      1.141
_refine_ls_R_factor_all          0.1953
_refine_ls_R_factor_obs          0.0700
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0801P)^2^+58.1816P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2273
_refine_ls_wR_factor_obs         0.1624
_reflns_number_observed          2542
_reflns_number_total             5545
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9702227_1.cif
_cod_data_source_block           IC9702227/3e
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0801P)^2^+58.1816P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0801P)^2^+58.1816P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        8039.6(25)
_cod_database_code               4323623