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_7216080
_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            'C198 H234 N36 Ni6 O12 S12'
_chemical_formula_weight         4047.19
_chemical_name_systematic
;
?
;
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 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                 95.7930(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.4822(2)
_cell_length_b                   27.7131(3)
_cell_length_c                   22.9061(3)
_cell_measurement_temperature    173(2)
_cell_volume                     10409.5(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0379
_diffrn_reflns_av_sigmaI/netI    0.0800
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            48083
_diffrn_reflns_theta_full        25.98
_diffrn_reflns_theta_max         25.98
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    0.717
_exptl_absorpt_correction_T_max  0.9515
_exptl_absorpt_correction_T_min  0.8411
_exptl_absorpt_correction_type   'semi-empirical '
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4260
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.940
_refine_diff_density_min         -0.594
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.011(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     2346
_refine_ls_number_reflns         30810
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_gt           0.0541
_refine_ls_shift/su_max          0.651
_refine_ls_shift/su_mean         0.026
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0686P)^2^+6.6114P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1188
_refine_ls_wR_factor_ref         0.1346
_reflns_number_gt                22987
_reflns_number_total             30810
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b419468c.txt
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      Pn
_cod_database_code               7216080