DPDS–DPS in situ transformation at room temperature via a 1,2-nucleophilic addition mechanism
De la Pinta, Noelia; Caballero, Ana B.; Madariaga, Gotzon; Ezpeleta, José M.; Rodriguez-Dieguez, Antonio; Salas, Juan M.; Cortés, Roberto; CrystEngComm 16 (2014) 8322–; doi:10.1039/C4CE00781F

data_7216463
_publ_section_title
;
 DPDS--DPS in situ transformation at room temperature via a
 1,2-nucleophilic addition mechanism
;
_journal_issue                   36
_journal_name_full               CrystEngComm
_journal_page_first              8322
_journal_paper_doi               10.1039/C4CE00781F
_journal_volume                  16
_journal_year                    2014
_chemical_formula_sum            'C40 H38 Cl2 N8 O11 S4 Zn'
_chemical_formula_weight         1071.35
_space_group_IT_number           92
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.529(2)
_cell_length_b                   16.529(2)
_cell_length_c                   16.604(2)
_cell_measurement_temperature    293(2)
_cell_volume                     4536.3(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_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  0.0397
_diffrn_reflns_av_sigmaI/netI    0.0308
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            28832
_diffrn_reflns_theta_full        28.20
_diffrn_reflns_theta_max         28.20
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    0.912
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2200
_exptl_crystal_size_max          0.0021
_exptl_crystal_size_mid          0.002
_exptl_crystal_size_min          0.002
_refine_diff_density_max         1.030
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.026(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         5315
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0460
_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^)+(0.0707P)^2^+3.2047P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1156
_refine_ls_wR_factor_ref         0.1195
_reflns_number_gt                4875
_reflns_number_total             5315
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ce00781f2.cif
_cod_data_source_block           an232
_cod_depositor_comments
'Adding full bibliography for 7216463--7216466.cif.'
_cod_original_cell_volume        4536.3(11)
_cod_original_sg_symbol_H-M      P41212
_cod_database_code               7216463