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_7206278
_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, C H4 O'
_chemical_formula_sum            'C37 H50 N2 O10'
_chemical_formula_weight         682.81
_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             11-01-20
_audit_creation_method           CRYSTALS_ver_14.07
_cell_angle_alpha                82.63(4)
_cell_angle_beta                 82.94(5)
_cell_angle_gamma                74.70(5)
_cell_formula_units_Z            2
_cell_length_a                   8.864(13)
_cell_length_b                   9.554(14)
_cell_length_c                   21.89(4)
_cell_measurement_reflns_used    3870
_cell_measurement_temperature    150
_cell_measurement_theta_max      32
_cell_measurement_theta_min      2
_cell_volume                     1766(5)
_computing_cell_refinement       'CrystalClear (Rigaku, 1997--2009)'
_computing_data_collection       'CrystalClear (Rigaku, 1997--2009)'
_computing_data_reduction        'CrystalClear (Rigaku, 1997--2009)'
_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 0.878
_diffrn_measured_fraction_theta_max 0.759
_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  0.070
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10117
_diffrn_reflns_theta_full        25.066
_diffrn_reflns_theta_max         32.982
_diffrn_reflns_theta_min         1.884
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.71
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku, 1997--2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             732.000
_exptl_crystal_size_max          0.061
_exptl_crystal_size_mid          0.014
_exptl_crystal_size_min          0.012
_refine_diff_density_max         0.46
_refine_diff_density_min         -0.47
_refine_ls_extinction_coef       660(160)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.0092
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     462
_refine_ls_number_reflns         4587
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.1223
_refine_ls_R_factor_gt           0.1070
_refine_ls_shift/su_max          0.0001663
_refine_ls_shift/su_mean         0.0000223
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.17P)^2^ + 4.32P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3010
_refine_ls_wR_factor_gt          0.2861
_refine_ls_wR_factor_ref         0.3010
_reflns_limit_h_max              12
_reflns_limit_h_min              -11
_reflns_limit_k_max              14
_reflns_limit_k_min              -14
_reflns_limit_l_max              32
_reflns_limit_l_min              0
_reflns_number_gt                3751
_reflns_number_total             10117
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.76
_oxford_diffrn_Wilson_scale      4.00
_oxford_refine_ls_r_factor_ref   0.1223
_oxford_refine_ls_scale          0.569(4)
_oxford_reflns_number_all        4587
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 046CJS10
_cod_data_source_file            c1ce05271c.txt
_cod_data_source_block           MeOH
_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               7206278