Temperature-, molar ratio- and counterion-effects on the crystal growth of bipyridinium-bis(alkylcarboxylic acid)?crown ether pseudorotaxanes
Mezei, Gellert; Kampf, Jeff W.; Pecoraro, Vincent L.; New Journal of Chemistry 31 (2007) 439–; doi:10.1039/b615273b

data_7052119
_publ_section_title
;
 Temperature-, molar ratio- and counterion-effects on the crystal
 growth of bipyridinium-bis(alkylcarboxylic acid)?crown ether
 pseudorotaxanes
;
_journal_issue                   3
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              439
_journal_paper_doi               10.1039/b615273b
_journal_volume                  31
_journal_year                    2007
_chemical_formula_moiety
;
C36 H44 O10, 2(C20 H26 N2 O4),
4(F6 P), 2(C2 H3 N)
;
_chemical_formula_sum            'C80 H102 F24 N6 O18 P4'
_chemical_formula_weight         2015.56
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.999(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.3358(19)
_cell_length_b                   16.055(2)
_cell_length_c                   20.135(3)
_cell_measurement_reflns_used    8424
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      23.93
_cell_measurement_theta_min      2.33
_cell_volume                     4533.0(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0561
_diffrn_reflns_av_sigmaI/netI    0.0285
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            8424
_diffrn_reflns_theta_full        24.50
_diffrn_reflns_theta_max         24.50
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    0.201
_exptl_absorpt_correction_T_max  0.9685
_exptl_absorpt_correction_T_min  0.9384
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Blessing, R. Acta Cryst. (1995) A51 33-38.
Sheldrick, G. SADABS (Version 2.10) Bruker/Siemens area
detector absorption and other corrections, University of
Gottingen, Germany 2003.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2088
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.572
_refine_diff_density_min         -0.402
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     602
_refine_ls_number_reflns         7516
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0436
_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^)+(0.0484P)^2^+4.1160P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1091
_refine_ls_wR_factor_ref         0.1192
_reflns_number_gt                5633
_reflns_number_total             7516
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b615273b.txt
_cod_data_source_block           Pseudorotaxane_IIb(gm08)
_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.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        4533.1(10)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7052119