Assessing dimerisation degree and cooperativity in a biomimetic small-molecule model by pulsed EPR
K. Ackermann; A. Giannoulis; D. B. Cordes; A. M. Z. Slawin; B. E. Bode; Chem.Commun. 51 (2015) 5257–; doi:10.1039/C4cc08656B

data_7116770
_publ_section_title
;
 Assessing dimerisation degree and cooperativity in a biomimetic
 small-molecule model by pulsed EPR
;
_journal_name_full               Chem.Commun.
_journal_page_first              5257
_journal_paper_doi               10.1039/C4cc08656B
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C44.5 H36 Cl N4 O3'
_chemical_formula_sum            'C44.5 H36 Cl N4 O3'
_chemical_formula_weight         710.25
_space_group_IT_number           86
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      86
_symmetry_space_group_name_Hall  '-P 4bc'
_symmetry_space_group_name_H-M   'P 42/n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2014-10-17 deposited with the CCDC.
2015-01-08 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.000
_cell_formula_units_Z            8
_cell_length_a                   36.726(11)
_cell_length_b                   36.726(13)
_cell_length_c                   5.6924(19)
_cell_measurement_reflns_used    3613
_cell_measurement_temperature    125
_cell_measurement_theta_max      74.50
_cell_measurement_theta_min      24.40
_cell_volume                     7678(4)
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b32'
_computing_data_collection
'CrystalClear-SM Expert 2.1 b32 (Rigaku, 2014)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b32'
_computing_molecular_graphics    'CrystalStructure 4.1'
_computing_publication_material  'CrystalStructure 4.1 (Rigaku, 2014)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR2011 (Burla, et al., 2012)'
_diffrn_ambient_temperature      125
_diffrn_detector_area_resol_mean 5.814
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.1388
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            59425
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         68.208
_diffrn_reflns_theta_min         2.406
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.237
_exptl_absorpt_correction_T_max  0.976
_exptl_absorpt_correction_T_min  0.440
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2976.00
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Chloroform/hexane'
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.65
_refine_diff_density_min         -0.67
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.612
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     527
_refine_ls_number_reflns         6909
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1648
_refine_ls_R_factor_gt           0.1365
_refine_ls_shift/su_max          0.084
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3766
_refine_ls_wR_factor_ref         0.4042
_reflns_number_gt                4822
_reflns_number_total             6909
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c4cc08656b2-2.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      'P 42/n'
_cod_database_code               7116770