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_7116769
_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         'C21 H21 I N O3'
_chemical_formula_sum            'C21 H21 I N O3'
_chemical_formula_weight         462.31
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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
_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                91.604(3)
_cell_angle_beta                 91.020(3)
_cell_angle_gamma                101.055(3)
_cell_formula_units_Z            12
_cell_length_a                   11.5839(13)
_cell_length_b                   15.7615(16)
_cell_length_c                   32.762(3)
_cell_measurement_reflns_used    6879
_cell_measurement_temperature    173
_cell_measurement_theta_max      12.70
_cell_measurement_theta_min      0.95
_cell_volume                     5866.7(10)
_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  'SHELXL2013 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2011 (Burla, et al., 2012)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 11.628
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            114568
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.389
_diffrn_reflns_theta_min         1.244
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.658
_exptl_absorpt_correction_T_max  0.890
_exptl_absorpt_correction_T_min  0.780
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2772.00
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Toluene'
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.89
_refine_diff_density_min         -0.84
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.868
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     1478
_refine_ls_number_reflns         21380
_refine_ls_number_restraints     108
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0267
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0547P)^2^+2.4315P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0924
_refine_ls_wR_factor_ref         0.1042
_reflns_number_gt                6712
_reflns_number_total             21380
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c4cc08656b2-2.cif
_cod_data_source_block           1
_cod_database_code               7116769
_shelx_res_checksum              98048