Carbene spacers in bis-porphyrinic scaffolds
Julien Haumesser; Jean-Paul Gisselbrecht; Jean Weiss; Romain Ruppert; Chem.Commun. 48 (2012) 11653–; doi:10.1039/c2cc36800e

data_7108627
_publ_section_title
;
 Carbene spacers in bis-porphyrinic scaffolds
;
_journal_name_full               Chem.Commun.
_journal_page_first              11653
_journal_paper_doi               10.1039/c2cc36800e
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety         'C104 H84 I2 N12 Ni2 O2 Pd'
_chemical_formula_sum            'C104 H84 I2 N12 Ni2 O2 Pd'
_chemical_formula_weight         2011.45
_chemical_name_systematic
;
?
;
_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                 109.885(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.311(3)
_cell_length_b                   26.899(5)
_cell_length_c                   13.696(2)
_cell_measurement_reflns_used    4893
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.39
_cell_measurement_theta_min      2.50
_cell_volume                     5650.8(17)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  triumph
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0828
_diffrn_reflns_av_sigmaI/netI    0.1272
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            39341
_diffrn_reflns_theta_full        27.83
_diffrn_reflns_theta_max         27.83
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    1.080
_exptl_absorpt_correction_T_max  0.9480
_exptl_absorpt_correction_T_min  0.6720
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.182
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
The residual electron density was assigned to two molecules of the
ethanol solvent [177/4= 44 e per asymmetric unit; two molecules of
C2H6O1 would give 52 e].
;
_refine_diff_density_max         2.549
_refine_diff_density_min         -0.960
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.958
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         13185
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.959
_refine_ls_R_factor_all          0.1655
_refine_ls_R_factor_gt           0.0887
_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^)+(0.1487P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2348
_refine_ls_wR_factor_ref         0.2684
_reflns_number_gt                6059
_reflns_number_total             13185
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c2cc36800e.txt
_cod_data_source_block           jwjh111128
_cod_original_cell_volume        5651.1(17)
_cod_original_sg_symbol_Hall     '-P 2ybc '
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_database_code               7108627