Dimeric self-association of an isophthalamide macrocycle in solution and the solid state
Serpell, Christopher J.; Thomas, Owen; Odell, Barbara; Claridge, Timothy D. W.; Chall, Ricky; Thompson, Amber L.; Beer, Paul D.; CrystEngComm 13 (2011) 4586–; doi:10.1039/c1ce05271c

data_7206277
_publ_section_title
;
 Dimeric self-association of an isophthalamide macrocycle in solution
 and the solid state
;
_journal_issue                   14
_journal_name_full               CrystEngComm
_journal_page_first              4586
_journal_paper_doi               10.1039/c1ce05271c
_journal_volume                  13
_journal_year                    2011
_chemical_formula_moiety         'C36 H46 N2 O9'
_chemical_formula_sum            'C36 H46 N2 O9'
_chemical_formula_weight         650.77
_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
_audit_creation_date             11-01-27
_audit_creation_method           CRYSTALS_ver_14.07
_cell_angle_alpha                68.6691(10)
_cell_angle_beta                 83.2934(9)
_cell_angle_gamma                70.4090(9)
_cell_formula_units_Z            2
_cell_length_a                   10.2724(2)
_cell_length_b                   13.2776(2)
_cell_length_c                   13.7434(3)
_cell_measurement_reflns_used    6675
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     1644.98(6)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 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 0.987
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.021
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23513
_diffrn_reflns_theta_full        26.287
_diffrn_reflns_theta_max         27.382
_diffrn_reflns_theta_min         5.233
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.80
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.250
_refine_diff_density_max         1.25
_refine_diff_density_min         -0.51
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9080
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         7343
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0658
_refine_ls_R_factor_gt           0.0560
_refine_ls_shift/su_max          0.0003834
_refine_ls_shift/su_mean         0.0000336
_refine_ls_structure_factor_coef Fsqd
_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:
114. 184. 108. 43.4 9.60
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1656
_refine_ls_wR_factor_gt          0.1558
_refine_ls_wR_factor_ref         0.1655
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              17
_reflns_limit_k_min              -15
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                6226
_reflns_number_total             7348
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.23
_oxford_diffrn_Wilson_scale      0.52
_oxford_refine_ls_r_factor_ref   0.0658
_oxford_refine_ls_scale          1.445(9)
_oxford_reflns_number_all        7344
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 010CJS11
_cod_data_source_file            c1ce05271c.txt
_cod_data_source_block           AntiAntiPolymorph
_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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               7206277