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_7206279
_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         '2(C36 H46 N2 O9), 0.5(C H2 Cl2)'
_chemical_formula_sum            'C36.5 H47 Cl N2 O9'
_chemical_formula_weight         693.23
_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             11-01-20
_audit_creation_method           CRYSTALS_ver_14.07
_cell_angle_alpha                108.7629(4)
_cell_angle_beta                 90.3014(4)
_cell_angle_gamma                102.0591(5)
_cell_formula_units_Z            4
_cell_length_a                   8.84420(10)
_cell_length_b                   18.9677(2)
_cell_length_c                   23.0861(3)
_cell_measurement_reflns_used    15895
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     3575.06(7)
_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    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.053
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            85693
_diffrn_reflns_theta_full        26.939
_diffrn_reflns_theta_max         27.488
_diffrn_reflns_theta_min         5.116
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.163
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.70
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1476
_exptl_crystal_size_max          0.900
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.49
_refine_diff_density_min         -1.70
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9709
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     884
_refine_ls_number_reflns         13862
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.1256
_refine_ls_R_factor_gt           0.0885
_refine_ls_shift/su_max          0.0002657
_refine_ls_shift/su_mean         0.0000263
_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:
57.2 87.7 41.8 9.93
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2828
_refine_ls_wR_factor_gt          0.2320
_refine_ls_wR_factor_ref         0.2828
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              23
_reflns_limit_k_min              -24
_reflns_limit_l_max              29
_reflns_limit_l_min              0
_reflns_number_gt                8889
_reflns_number_total             16246
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.93
_oxford_diffrn_Wilson_scale      5.71
_oxford_refine_ls_r_factor_ref   0.1255
_oxford_refine_ls_scale          0.4489(10)
_oxford_reflns_number_all        13864
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 023CJS09
_cod_data_source_file            c1ce05271c.txt
_cod_data_source_block           DCM
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C36.50 H47 Cl1 N2 O9'
_cod_database_code               7206279