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_7206281
_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, 0.5(C3 H6 O)'
_chemical_formula_sum            'C37.5 H49 N2 O9.5'
_chemical_formula_weight         679.81
_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             11-01-12
_audit_creation_method           CRYSTALS_ver_14.07
_cell_angle_alpha                101.3301(13)
_cell_angle_beta                 102.2021(14)
_cell_angle_gamma                95.3807(12)
_cell_formula_units_Z            4
_cell_length_a                   11.2663(3)
_cell_length_b                   14.6885(5)
_cell_length_c                   22.7937(7)
_cell_measurement_reflns_used    12983
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     3578.74(19)
_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 0.970
_diffrn_measured_fraction_theta_max 0.934
_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  0.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            42050
_diffrn_reflns_theta_full        25.155
_diffrn_reflns_theta_max         27.642
_diffrn_reflns_theta_min         5.185
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.091
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.90
_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    1.262
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.35
_refine_diff_density_min         -0.29
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0746
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     911
_refine_ls_number_reflns         6440
_refine_ls_number_restraints     54
_refine_ls_R_factor_all          0.1387
_refine_ls_R_factor_gt           0.0663
_refine_ls_shift/su_max          0.0004712
_refine_ls_shift/su_mean         0.0000191
_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:
1.29 1.11 1.33 0.388 0.379
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0938
_refine_ls_wR_factor_gt          0.0587
_refine_ls_wR_factor_ref         0.0587
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              18
_reflns_limit_k_min              -19
_reflns_limit_l_max              29
_reflns_limit_l_min              0
_reflns_number_gt                6440
_reflns_number_total             15566
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.94
_oxford_diffrn_Wilson_scale      23.09
_oxford_refine_ls_r_factor_ref   0.0663
_oxford_refine_ls_scale          0.2425(4)
_oxford_reflns_number_all        11601
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_oxford_structure_analysis_title 5851
_cod_data_source_file            c1ce05271c.txt
_cod_data_source_block           Acetone
_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_original_formula_sum        'C37.50 H49 N2 O9.50'
_cod_database_code               7206281