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_4505058
_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            'C81 H86 N17 Ni2 O14 S4'
_chemical_formula_weight         1767.33
_chemical_name_systematic
; 
 cis-[Ni(L-S,O)(pyridine)2]2. pyridine/water solvate 
;
_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                97.30(3)
_cell_angle_beta                 100.30(3)
_cell_angle_gamma                100.52(3)
_cell_formula_units_Z            1
_cell_length_a                   9.4807(19)
_cell_length_b                   12.993(3)
_cell_length_c                   18.474(4)
_cell_measurement_temperature    173(2)
_cell_volume                     2171.2(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0573
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            11143
_diffrn_reflns_theta_full        28.68
_diffrn_reflns_theta_max         28.68
_diffrn_reflns_theta_min         2.29
_exptl_absorpt_coefficient_mu    0.601
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.7533
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             923
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.50
_refine_diff_density_max         1.004
_refine_diff_density_min         -0.827
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     538
_refine_ls_number_reflns         11143
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0890
_refine_ls_R_factor_gt           0.0508
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0604P)^2^+1.4724P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1185
_refine_ls_wR_factor_ref         0.1345
_reflns_number_gt                7637
_reflns_number_total             11143
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg049877qsi20040402_093600.cif
_cod_data_source_block           2
_cod_original_cell_volume        2171.1(8)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4505058