Anion-dependent crystallization of zinc complexes with the ligand 4′,5′-diaza-9′-(4,5-disubstituted-1,3-dithiol-2-ylidene) fluorene: Structures and spectroscopic properties
Zhu, Qin-Yu; Yu, Lei; Qin, Yu-Rong; Huo, Li-Bin; Shao, Ming-Yan; Dai, Jie; CrystEngComm 13 (2011) 2521–; doi:10.1039/c0ce00424c

data_7205597
_publ_section_title
;
 Anion-dependent crystallization of zinc complexes with the ligand
 4&#x2032;,5&#x2032;-diaza-9&#x2032;-(4,5-disubstituted-1,3-dithiol-2-ylidene)
 fluorene: Structures and spectroscopic properties
;
_journal_issue                   7
_journal_name_full               CrystEngComm
_journal_page_first              2521
_journal_paper_doi               10.1039/c0ce00424c
_journal_volume                  13
_journal_year                    2011
_chemical_formula_sum            'C50 H44 Cl8 N6 O2 S12 Zn3'
_chemical_formula_weight         1625.42
_chemical_name_systematic
;
?
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      13
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/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                 96.552(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.410(4)
_cell_length_b                   11.2071(15)
_cell_length_c                   23.501(4)
_cell_measurement_reflns_used    19189
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.6
_cell_measurement_theta_min      3.0
_cell_volume                     6648.7(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_sigmaI/netI    0.0660
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            30896
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.14
_exptl_absorpt_coefficient_mu    1.812
_exptl_absorpt_correction_T_max  0.7132
_exptl_absorpt_correction_T_min  0.4643
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3208
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.462
_refine_diff_density_min         -1.439
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.185
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     743
_refine_ls_number_reflns         11232
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.192
_refine_ls_R_factor_all          0.1176
_refine_ls_R_factor_gt           0.1033
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0002P)^2^+42.3529P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1797
_refine_ls_wR_factor_ref         0.1862
_reflns_number_gt                9430
_reflns_number_total             11232
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0ce00424c.txt
_cod_data_source_block           3
_cod_original_cell_volume        6648.7(17)
_cod_original_sg_symbol_H-M      'P 2/c'
_cod_database_code               7205597