Design, synthesis, structural analysis and atropoisomerisation studies of polynucleating ligands based on porphyrins bearing catechol units
Zimmer, Bertrand; Bulach, Véronique; Drexler, Cathy; Erhardt, Sabine; Hosseini, Mir Wais; De Cian, André; New Journal of Chemistry 26 (2002) 43–57; doi:10.1039/b104084g

data_7050677
_publ_section_title
;
 Design, synthesis, structural analysis and atropoisomerisation studies
 of polynucleating ligands based on porphyrins bearing catechol units
;
_journal_issue                   1
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              43
_journal_page_last               57
_journal_paper_doi               10.1039/b104084g
_journal_volume                  26
_journal_year                    2002
_chemical_formula_moiety         'C76 H66 N8 O16'
_chemical_formula_sum            'C76 H66 N8 O16'
_chemical_formula_weight         1347.42
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.2498(5)
_cell_length_b                   22.2498(5)
_cell_length_c                   13.3040(4)
_cell_measurement_reflns_used    19284
_cell_measurement_temperature    173
_cell_measurement_theta_max      32.5
_cell_measurement_theta_min      1.4
_cell_volume                     6586.2(3)
_computing_publication_material  CIFGEN_IN_OpenMoleN_(_1997)
_computing_structure_refinement  LSFM_OpenMoleN_(_1997)
_computing_structure_solution    Direct_methods_(SIR,_Burla_et_al.,_1989)
_diffrn_ambient_temperature      173
_diffrn_measurement_details
;
19284 reflections were collected using program Collect
("Collect" Data collection software, Nonius B.V., 1998)
The conditions were as follow : crystal to detector distance =  30. mm.
Scan angle =  2.0 deg 1 scans of   60 sec per frame.
Data collection was divided into  1 set(s)
with the following starting angles and number of frames :

Set 1 Theta =    6.90 Omega =    0.00 Kappa =    0.00   69 frames
Friedel pairs were averaged. Internal R = 0.05
;
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\p scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.050
_diffrn_reflns_av_sigmaI/netI    0.333
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            19284
_diffrn_reflns_theta_max         32.47
_diffrn_reflns_theta_min         2.5
_diffrn_source                   xray_tube
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.097
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.36
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             2824
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.228
_refine_diff_density_min         -0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.523
_refine_ls_goodness_of_fit_ref   1.344
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3132
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.116
_refine_ls_R_factor_gt           0.062
_refine_ls_shift/esd_mean        0.000
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.087
_refine_ls_wR_factor_ref         0.074
_reflns_number_gt                3132
_reflns_number_total             5633
_reflns_threshold_expression     >3.0\s(I)
_cod_data_source_file            b104084g.txt
_cod_data_source_block           st350
_cod_original_cell_volume        6586.2(5)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               7050677