Axially Chiral β,β'-Bisporphyrins: Synthesis and Configurational Stability Tuned by the Central Metals
Bringmann, Gerhard; Götz, Daniel C. G.; Gulder, Tobias A. M.; Gehrke, Tim H.; Bruhn, Torsten; Kupfer, Thomas; Radacki, Krzysztof; Braunschweig, Holger; Heckmann, Alexander; Lambert, Christoph; Journal of the American Chemical Society 130 (2008) 17812–17825; doi:10.1021/ja8055886

data_4121936
_publ_section_title
;
 Axially Chiral \b,\b'-Bisporphyrins: Synthesis and Configurational
 Stability Tuned by the Central Metals
;
_journal_coden_ASTM              JACSAT
_journal_issue                   52
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17812
_journal_page_last               17825
_journal_paper_doi               10.1021/ja8055886
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C50 H39 B Cu N4 O2, 2(C6 H6)'
_chemical_formula_sum            'C62 H51 B Cu N4 O2'
_chemical_formula_weight         958.42
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.916(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.2094(9)
_cell_length_b                   10.8327(5)
_cell_length_c                   24.9242(12)
_cell_measurement_reflns_used    9895
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.79
_cell_measurement_theta_min      2.29
_cell_volume                     4869.6(4)
_computing_cell_refinement       'Saint+ ver. 7.12A (Bruker AXS)'
_computing_data_collection       'APEX2 ver. 1.0-27 (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. 7.12A (Bruker AXS)'
_computing_molecular_graphics    'XP ver. 5.1 (Bruker AXS, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0659
_diffrn_reflns_av_sigmaI/netI    0.0559
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            66500
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.04
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    0.499
_exptl_absorpt_correction_T_max  0.961
_exptl_absorpt_correction_T_min  0.889
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs 2004/1 (Brucker Nonius 2004)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2004
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.706
_refine_diff_density_min         -0.584
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         9544
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0905
_refine_ls_R_factor_gt           0.0605
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0633P)^2^+7.4069P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1451
_refine_ls_wR_factor_ref         0.1588
_reflns_number_gt                7062
_reflns_number_total             9544
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             4108922
_cod_data_source_file            ja8055886_si_001.cif
_cod_data_source_block           Cu097
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Updated bibliographic information.

 Antanas Vaitkus,
 2019-09-19

 Marked entry as a duplicate of entry 4108922.

 Antanas Vaitkus,
 2019-09-19
;
_cod_original_sg_symbol_Hall     '-P 2ybc '
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4121936