Unusual conformational preference of an aromatic secondary urea: solvent-dependent open-closed conformational switching of N,N'-bis(porphyrinyl)urea
Mio Matsumura; Aya Tanatani; Isao Azumaya; Hyuma Masu; Daisuke Hashizume; Hiroyuki Kagechika; Atsuya Muranaka; Masanobu Uchiyama; Chem.Commun. 49 (2013) 2290–; doi:10.1039/c2cc37583d

data_7108942
_publ_section_title
;
 Unusual conformational preference of an aromatic secondary urea:
 solvent-dependent open-closed conformational switching of
 N,N'-bis(porphyrinyl)urea
;
_journal_name_full               Chem.Commun.
_journal_page_first              2290
_journal_paper_doi               10.1039/c2cc37583d
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety         'C73 H88 N10 Ni2 O, 2(C H Cl3)'
_chemical_formula_sum            'C75 H90 Cl6 N10 Ni2 O'
_chemical_formula_weight         1477.69
_chemical_name_systematic
;
?
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.8849(4)
_cell_length_b                   14.7428(3)
_cell_length_c                   28.8660(7)
_cell_measurement_reflns_used    177035
_cell_measurement_temperature    90
_cell_measurement_theta_max      34.30
_cell_measurement_theta_min      1.21
_cell_volume                     7185.6(3)
_computing_cell_refinement       HKL2000
_computing_data_collection       CrystalClear
_computing_data_reduction        HKL2000
_computing_molecular_graphics    'ORTEP-3 for Windows'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  SHELXL-97
_computing_structure_solution    SIR2004
_diffrn_ambient_temperature      90
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Rigaku AFC-8 with Saturn70 CCD'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0897
_diffrn_reflns_av_sigmaI/netI    0.0300
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            167863
_diffrn_reflns_theta_full        30.09
_diffrn_reflns_theta_max         30.09
_diffrn_reflns_theta_min         1.86
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.799
_exptl_absorpt_correction_T_max  0.86603
_exptl_absorpt_correction_T_min  0.78544
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
MULABS - Empirical Correction for Absorption Anisotropy.
R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3104
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.826
_refine_diff_density_min         -0.931
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     498
_refine_ls_number_reflns         10416
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.180
_refine_ls_R_factor_all          0.0900
_refine_ls_R_factor_gt           0.0721
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0568P)^2^+22.7580P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1887
_refine_ls_wR_factor_ref         0.1990
_reflns_number_gt                8208
_reflns_number_total             10416
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c2cc37583d.txt
_cod_data_source_block           MM2-186-1
_cod_database_code               7108942