Synthesis and structural characterisation of novel bimetallic dipyrromethene complexes: rotational locking of the 5-aryl group.
Sutton, Jonathan M; Rogerson, Eleanor; Wilson, Christopher J; Sparke, Amanda E; Archibald, Stephen J; Boyle, Ross W; Chemical communications (Cambridge, England)  (2004) 1328–1329; doi:10.1039/b404147j

data_7102665
_publ_section_title
;
 Synthesis and structural characterisation of novel bimetallic
 dipyrromethene complexes: rotational locking of the 5-aryl group.
;
_journal_issue                   11
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              1328
_journal_page_last               1329
_journal_paper_doi               10.1039/b404147j
_journal_year                    2004
_chemical_formula_sum            'C46 H58 N6 O6 S2 Zn2'
_chemical_formula_weight         985.84
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 98.061(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.9761(19)
_cell_length_b                   8.9847(8)
_cell_length_c                   19.804(3)
_cell_measurement_temperature    150(2)
_cell_volume                     2286.1(5)
_computing_cell_refinement       X-AREA
_computing_data_collection       X-AREA
_computing_data_reduction        X-RED
_computing_molecular_graphics    'ORTEP II (Johnson, 1976)'
_computing_publication_material  'SHELXL 97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Stoe IPDSII image plate'
_diffrn_measurement_method
'135 frames at 1^o intervals, exposure time 1 minutes'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0584
_diffrn_reflns_av_sigmaI/netI    0.0754
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            28786
_diffrn_reflns_theta_full        33.53
_diffrn_reflns_theta_max         33.53
_diffrn_reflns_theta_min         2.49
_exptl_absorpt_coefficient_mu    1.195
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.200
_refine_diff_density_min         -0.934
_refine_diff_density_rms         0.110
_refine_ls_extinction_coef       0.0074(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.878
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         8884
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.878
_refine_ls_R_factor_all          0.0987
_refine_ls_R_factor_gt           0.0548
_refine_ls_shift/su_max          0.034
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0938P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1381
_refine_ls_wR_factor_ref         0.1532
_reflns_number_gt                4827
_reflns_number_total             8884
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b404147j.txt
_cod_data_source_block           sja3_01
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7102665