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_7206280
_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, C6 F5 I'
_chemical_formula_sum            'C42 H46 F5 I N2 O9'
_chemical_formula_weight         944.73
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                90
_cell_angle_beta                 110.460(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   50.61(3)
_cell_length_b                   9.703(6)
_cell_length_c                   19.082(11)
_cell_measurement_reflns_used    15684
_cell_measurement_temperature    150
_cell_measurement_theta_max      63
_cell_measurement_theta_min      2
_cell_volume                     8779(9)
_computing_cell_refinement       'CrystalClear (Rigaku, 1997--2002)'
_computing_data_collection       'CrystalClear (Rigaku, 1997--2002)'
_computing_data_reduction        'CrystalClear (Rigaku, 1997--2002)'
_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 0.997
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_device       Serial
_diffrn_measurement_device_type  Unknown
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  'Si(1 1 1) double-crystal monochromator'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_reflns_av_R_equivalents  0.108
_diffrn_reflns_limit_h_max       68
_diffrn_reflns_limit_h_min       -76
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            50232
_diffrn_reflns_theta_full        29.492
_diffrn_reflns_theta_max         31.712
_diffrn_reflns_theta_min         0.832
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.290
_exptl_absorpt_correction_T_max  0.80
_exptl_absorpt_correction_T_min  0.40
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku, 1997--2002)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3856.000
_exptl_crystal_size_max          0.368
_exptl_crystal_size_mid          0.051
_exptl_crystal_size_min          0.034
_refine_diff_density_max         0.82
_refine_diff_density_min         -0.73
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.2305
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     832
_refine_ls_number_reflns         3934
_refine_ls_number_restraints     1387
_refine_ls_R_factor_all          0.1126
_refine_ls_R_factor_gt           0.0917
_refine_ls_shift/su_max          0.0007897
_refine_ls_shift/su_mean         0.0000487
_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:
12.5 4.86 9.46 3.25
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1154
_refine_ls_wR_factor_gt          0.1028
_refine_ls_wR_factor_ref         0.1028
_reflns_limit_h_max              68
_reflns_limit_h_min              -76
_reflns_limit_k_max              14
_reflns_limit_k_min              0
_reflns_limit_l_max              28
_reflns_limit_l_min              0
_reflns_number_gt                3934
_reflns_number_total             14914
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   4.91
_oxford_diffrn_Wilson_scale      2.16
_oxford_refine_ls_r_factor_ref   0.0917
_oxford_refine_ls_scale          0.824(3)
_oxford_reflns_number_all        5110
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_oxford_structure_analysis_title 005CJS10
_cod_data_source_file            c1ce05271c.txt
_cod_data_source_block           C6F5I
_cod_original_sg_symbol_H-M      'C 2/c '
_cod_original_formula_sum        'C42 H46.00 F5 I1 N2 O9'
_cod_database_code               7206280