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_7050678
_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         'C149 H110 Cl10 N16 O24'
_chemical_formula_sum            'C149 H110 Cl10 N16 O24'
_chemical_formula_weight         2863.16
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_date             20-06-00
_cell_angle_alpha                90
_cell_angle_beta                 92.368(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.7436(2)
_cell_length_b                   12.9855(3)
_cell_length_c                   39.3596(9)
_cell_measurement_reflns_used    15305
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.4
_cell_volume                     6507.7(2)
_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
;
15305 reflections were collected using program Collect
("Collect" Data collection software, Nonius B.V., 1998)
The conditions were as follow : crystal to detector distance =  47. mm.
Scan angle =  0.8 deg 1 scans of  120 sec per frame.
Data collection was divided into  2 set(s)
with the following starting angles and number of frames :

Set 1 Theta =   10.10 Omega =    0.00 Kappa =    0.00  249 frames
Set 2 Theta =   -9.90 Kappa =  -68.00 Phi   =    0.00  118 frames
Friedel pairs were averaged. Internal R = 0.04
;
_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  0.040
_diffrn_reflns_av_sigmaI/netI    0.333
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            15305
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.5
_diffrn_source                   xray_tube
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.297
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.46
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             2956
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.589
_refine_diff_density_min         -0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   7.546
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     911
_refine_ls_number_reflns         7282
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.165
_refine_ls_R_factor_gt           0.071
_refine_ls_shift/esd_mean        0.000
_refine_ls_shift/su_max          0.006
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 4Fo^2^/(\s^2^(Fo^2^)+0.0004 Fo^4^)+0.2'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.391
_refine_ls_wR_factor_ref         0.082
_reflns_number_gt                7282
_reflns_number_total             15305
_reflns_threshold_expression     >3.0\s(I)
_cod_data_source_file            b104084g.txt
_cod_data_source_block           st647
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '4Fo^2^/(\s^2^(Fo^2^)+0.0004
Fo^4^)+0.2' was changed to 'calc'. New tag
'_refine_ls_weighting_details' was created. The value of the new tag
was set to 'w = 4Fo^2^/(\s^2^(Fo^2^)+0.0004 Fo^4^)+0.2'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_cell_volume        6507.7(4)
_cod_database_code               7050678