Grid-double-helicate interconversion
Adrian-Mihail Stadler; Christophe Burg; Juan Ramirez; Jean-Marie Lehn; Chem.Commun. 49 (2013) 5733–; doi:10.1039/c3cc38580a

data_7109393
_publ_section_title
;
 Grid-double-helicate interconversion
;
_journal_name_full               Chem.Commun.
_journal_page_first              5733
_journal_paper_doi               10.1039/c3cc38580a
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety         'C96 H88 Cu4 N32, 8(C F3 O3 S), 5(C H3 N O2)'
_chemical_formula_sum            'C109 H103 Cu4 F24 N37 O34 S8'
_chemical_formula_weight         3441.92
_chemical_name_systematic
;
?
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 111.0630(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.5751(10)
_cell_length_b                   44.611(3)
_cell_length_c                   19.3360(12)
_cell_measurement_reflns_used    9912
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      2.44
_cell_volume                     14147.3(15)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  triumph
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0514
_diffrn_reflns_av_sigmaI/netI    0.0643
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       62
_diffrn_reflns_limit_k_min       -62
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            114606
_diffrn_reflns_theta_full        30.10
_diffrn_reflns_theta_max         30.10
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    0.830
_exptl_absorpt_correction_T_max  0.8856
_exptl_absorpt_correction_T_min  0.7324
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             6992
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
The residual electron density was assigned to three molecules of the
nitromethane solvent [447/4= 112 e per asymmetric unit; three molecules
of C1H3N1O2 would give 96 e].
;
_refine_diff_density_max         1.809
_refine_diff_density_min         -1.697
_refine_diff_density_rms         0.143
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.363(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1502
_refine_ls_number_reflns         36244
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.1256
_refine_ls_R_factor_gt           0.0920
_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^)+(0.1901P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2495
_refine_ls_wR_factor_ref         0.2745
_reflns_number_gt                23255
_reflns_number_total             36244
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c3cc38580a.txt
_cod_data_source_block           Cu4L4_CF3SO3_8_CH3NO2_5
_cod_original_cell_volume        14147.2(14)
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               7109393