Metallamacrocyclic complexes of Ni(ii) with 3,3,3?,3?-tetraalkyl-1,1?-aroylbis(thioureas): crystal and molecular structures of a 2 : 2 metallamacrocycle and a pyridine adduct of the analogous 3 : 3 complex
Hallale, Oren; Bourne, Susan A.; Koch, Klaus R.; CrystEngComm 7 (2005) 161–; doi:10.1039/b419468c

data_7216079
_publ_section_title
;
 Metallamacrocyclic complexes of Ni(ii) with
 3,3,3?,3?-tetraalkyl-1,1?-aroylbis(thioureas): crystal and molecular
 structures of a 2 : 2 metallamacrocycle and a pyridine adduct of the
 analogous 3 : 3 complex
;
_journal_issue                   25
_journal_name_full               CrystEngComm
_journal_page_first              161
_journal_paper_doi               10.1039/b419468c
_journal_volume                  7
_journal_year                    2005
_chemical_formula_sum            'C18 H24 N4 Ni O2 S2'
_chemical_formula_weight         451.24
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                81.0900(10)
_cell_angle_beta                 82.7990(10)
_cell_angle_gamma                84.6010(10)
_cell_formula_units_Z            2
_cell_length_a                   8.32370(10)
_cell_length_b                   9.61490(10)
_cell_length_c                   12.87170(10)
_cell_measurement_temperature    173(2)
_cell_volume                     1006.749(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0147
_diffrn_reflns_av_sigmaI/netI    0.0254
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8648
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    1.192
_exptl_absorpt_correction_T_max  0.8415
_exptl_absorpt_correction_T_min  0.7163
_exptl_absorpt_correction_type   semi-empirical
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             472
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.356
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.773
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         4625
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.773
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0246
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0855
_refine_ls_wR_factor_ref         0.0924
_reflns_number_gt                4139
_reflns_number_total             4625
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b419468c.txt
_cod_data_source_block           1
_cod_original_cell_volume        1006.750(18)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7216079