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_7206282
_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, 1.75(C2 H3 N)'
_chemical_formula_sum            'C39.5 H51.25 N3.75 O9'
_chemical_formula_weight         722.61
_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                102.6195(4)
_cell_angle_beta                 92.0868(4)
_cell_angle_gamma                113.4947(4)
_cell_formula_units_Z            4
_cell_length_a                   13.56390(10)
_cell_length_b                   16.22440(10)
_cell_length_c                   19.8583(2)
_cell_measurement_reflns_used    16883
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     3873.60(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    'USER DEFINED STRUCTURE SOLUTION'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.988
_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       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            76597
_diffrn_reflns_theta_full        26.384
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         5.127
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_T_max  0.96
_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            colourless
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1546.000
_exptl_crystal_size_max          0.520
_exptl_crystal_size_mid          0.510
_exptl_crystal_size_min          0.500
_refine_diff_density_max         1.40
_refine_diff_density_min         -0.77
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9236
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     983
_refine_ls_number_reflns         14981
_refine_ls_number_restraints     54
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0562
_refine_ls_shift/su_max          0.0004277
_refine_ls_shift/su_mean         0.0000332
_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:
79.9 128. 73.8 29.3 6.59
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1441
_refine_ls_wR_factor_gt          0.1368
_refine_ls_wR_factor_ref         0.1439
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              20
_reflns_limit_k_min              -21
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                12736
_reflns_number_total             17567
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.68
_oxford_diffrn_Wilson_scale      1.77
_oxford_refine_ls_r_factor_ref   0.0661
_oxford_refine_ls_scale          0.8629(18)
_oxford_reflns_number_all        14987
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 033CJS08
_cod_data_source_file            c1ce05271c.txt
_cod_data_source_block           MeCN
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C39.50 H51.25 N3.75 O9'
_cod_database_code               7206282