Interlocked Host Anion Recognition by an Indolocarbazole-Containing [2]Rotaxane
Asha Brown; Kathleen M. Mullen; Jay Ryu; Michał J. Chmielewski; Sérgio M. Santos; Vitor Felix; Amber L. Thompson; John E. Warren; Sofia I. Pascu; Paul D. Beer; Journal of the American Chemical Society 131 (2009) 4937–4952; doi:10.1021/ja809905x

data_4104136
_publ_contact_author             'Paul D. Beer'
_publ_contact_author_email       paul.beer@chem.ox.ac.uk
_publ_section_title
;
 Interlocked Host Anion Recognition by an Indolocarbazole-Containing
 [2]Rotaxane
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4937
_journal_page_last               4952
_journal_paper_doi               10.1021/ja809905x
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C42 H42 N6 O2, 4(P F6), 2(C2 H3 N)'
_chemical_formula_sum            'C46 H48 F24 N8 O2 P4'
_chemical_formula_weight         1324.79
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             08-05-28
_audit_creation_method           CRYSTALS_ver_12.85
_cell_angle_alpha                90
_cell_angle_beta                 107.8184(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.8889(2)
_cell_length_b                   8.28350(10)
_cell_length_c                   29.5789(3)
_cell_measurement_reflns_used    12540
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     5572.41(10)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.070
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            57624
_diffrn_reflns_theta_full        26.903
_diffrn_reflns_theta_max         27.452
_diffrn_reflns_theta_min         5.114
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.262
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.64
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            clear_pale_colourless
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2688
_exptl_crystal_size_max          1.00
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.66
_refine_diff_density_min         -0.62
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.9625
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     545
_refine_ls_number_reflns         6695
_refine_ls_number_restraints     817
_refine_ls_R_factor_all          0.1427
_refine_ls_R_factor_gt           0.0737
_refine_ls_shift/su_max          0.000461
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 1.53 1.18 1.35 0.291 0.283 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1133
_refine_ls_wR_factor_gt          0.0739
_refine_ls_wR_factor_ref         0.0739
_reflns_limit_h_max              29
_reflns_limit_h_min              -30
_reflns_limit_k_max              10
_reflns_limit_k_min              0
_reflns_limit_l_max              38
_reflns_limit_l_min              0
_reflns_number_gt                6695
_reflns_number_total             12568
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.91
_oxford_diffrn_Wilson_scale      28.96
_oxford_refine_ls_r_factor_ref   0.0737
_oxford_refine_ls_scale          0.2418(4)
_oxford_reflns_number_all        12567
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_oxford_structure_analysis_title 5631
_cod_data_source_file            ja809905x_si_002_2.cif
_cod_data_source_block           macrocycle-1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' 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 
;
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_database_code               4104136