Hydrogen-Bonding Networks in a Bipodal Acyl-thiourea and Its NiII2:2 Metallamacrocyclic Complex
Bourne, Susan A.; Hallale, Oren; Koch, Klaus R.; Crystal Growth & Design 5 (2005) 307–; doi:10.1021/cg049877q

data_4505057
_publ_section_title
;
 Hydrogen-Bonding Networks in a Bipodal Acyl-thiourea and Its NiII2:2
 Metallamacrocyclic Complex
;
_journal_issue                   1
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              307
_journal_paper_doi               10.1021/cg049877q
_journal_volume                  5
_journal_year                    2005
_chemical_formula_sum            'C18 H26 N4 O6 S2'
_chemical_formula_weight         458.56
_chemical_name_systematic
; 
 3,3,3',3'-tetra(2-hydroxyethyl)-1,1'-isophthaloylbis(thiourea) 
;
_space_group_IT_number           96
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4nw 2abw'
_symmetry_space_group_name_H-M   'P 43 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                   9.2890(13)
_cell_length_b                   9.2890(13)
_cell_length_c                   25.028(5)
_cell_measurement_temperature    193(2)
_cell_volume                     2159.6(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  diffractometer
_diffrn_measurement_method       'phi and omega scans'
_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  0.0266
_diffrn_reflns_av_sigmaI/netI    0.0167
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            12620
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         3.93
_exptl_absorpt_coefficient_mu    0.289
_exptl_absorpt_correction_T_max  0.8931
_exptl_absorpt_correction_T_min  0.8457
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.169
_refine_diff_density_min         -0.185
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     149
_refine_ls_number_reflns         2660
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0266
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+0.2585P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0736
_refine_ls_wR_factor_ref         0.0753
_reflns_number_gt                2589
_reflns_number_total             2660
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg049877qsi20040402_093600.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      P4(3)2(1)2
_cod_database_code               4505057