Synthesis of New Porphyrins with Peripheral Conjugated Chelates and Their Use for the Preparation of Porphyrin Dimers Linked by Metal Ions
Sébastien Richeter; Christophe Jeandon; Jean-Paul Gisselbrecht; Roland Graff; Romain Ruppert; Henry J. Callot; Inorganic Chemistry 43 (2004) 251–263; doi:10.1021/ic035203d

data_4310362
_publ_section_title
;
 Synthesis of New Porphyrins with Peripheral Conjugated Chelates and Their
 Use for the Preparation of Porphyrin Dimers Linked by Metal Ions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              251
_journal_page_last               263
_journal_paper_doi               10.1021/ic035203d
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         'C91 H58 Cl2 N10 Ni2 O3'
_chemical_formula_sum            'C91 H58 Cl2 N10 Ni2 O3'
_chemical_formula_weight         1527.87
_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             1-10-02
_cell_angle_alpha                90
_cell_angle_beta                 107.796(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   22.5313(3)
_cell_length_b                   9.6798(2)
_cell_length_c                   17.6195(6)
_cell_measurement_reflns_used    16565
_cell_measurement_temperature    173
_cell_measurement_theta_max      29.1
_cell_measurement_theta_min      1.4
_cell_volume                     3658.91(18)
_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
;
   16565 reflections were collected using program Collect
  ("Collect" Data collection software, Nonius B.V., 1998)
  The conditions were as follow : crystal to detector distance =  36. mm.
  Scan angle =  1.6 deg 1 scans of   60 sec per frame.
  Data collection was divided into  2 set(s)
  with the following starting angles and number of frames :
  Set 1 Theta =    7.80 Omega =    0.00 Kappa =    0.00  139 frames
  Set 2 Theta =   -5.80 Kappa = -170.00 Phi   =    0.00   34 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       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            16565
_diffrn_reflns_theta_max         29.13
_diffrn_reflns_theta_min         2.5
_diffrn_source                   xray_tube
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.649
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.39
_exptl_crystal_density_method    none
_exptl_crystal_description       needle
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.183
_refine_diff_density_min         -0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   3.743
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     505
_refine_ls_number_reflns         5232
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.111
_refine_ls_R_factor_gt           0.052
_refine_ls_shift/esd_mean        0.001
_refine_ls_shift/su_max          0.016
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.221
_refine_ls_wR_factor_ref         0.070
_reflns_number_gt                5232
_reflns_number_total             10349
_reflns_threshold_expression     >3.0\s(I)
_cod_data_source_file            ic035203dsi20031020_110310.cif
_cod_data_source_block           st1244
_cod_depositor_comments
;
 Marking attached hydrogen atoms.

 Antanas Vaitkus,
 2018-01-29
;
_cod_original_cell_volume        3658.9(2)
_cod_database_code               4310362