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_7052118
_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), 2(P F6), 2(H2 O4 P), C2 H3 N, H2 O
;
_chemical_formula_sum            'C78 H105 F12 N5 O27 P4'
_chemical_formula_weight         1896.55
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                85.446(8)
_cell_angle_beta                 83.877(7)
_cell_angle_gamma                70.685(7)
_cell_formula_units_Z            2
_cell_length_a                   13.6418(16)
_cell_length_b                   16.700(2)
_cell_length_c                   20.050(2)
_cell_measurement_reflns_used    5912
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      21.04
_cell_measurement_theta_min      2.35
_cell_volume                     4281.3(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART-1K'
_computing_data_reduction        'Bruker SAINT'
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0872
_diffrn_reflns_av_sigmaI/netI    0.0498
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            86695
_diffrn_reflns_theta_full        22.70
_diffrn_reflns_theta_max         22.70
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    0.196
_exptl_absorpt_correction_T_max  0.9807
_exptl_absorpt_correction_T_min  0.9693
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1984
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.970
_refine_diff_density_min         -0.522
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1152
_refine_ls_number_reflns         11395
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.1011
_refine_ls_R_factor_gt           0.0627
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0817P)^2^+10.6380P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1530
_refine_ls_wR_factor_ref         0.1777
_reflns_number_gt                7850
_reflns_number_total             11395
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b615273b.txt
_cod_data_source_block           Pseudorotaxane_IIa(gm07)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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        4281.4(9)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7052118