Isolated Magnetic Clusters of Co(II) and Ni(II) within 3-Dimensional Organic Frameworks of 6-Mercaptonicotinic Acid: Unique Structural Topologies Based on Selectivity for Hard and Soft Coordination Environments
Simon M. Humphrey; Richard A. Mole; Mary McPartlin; Eric J. L. McInnes; Paul T. Wood; Inorganic Chemistry 44 (2005) 5981–5983; doi:10.1021/ic050768q

data_4309462
_publ_section_title
;
Isolated Magnetic Clusters of Co(II) and Ni(II) within 3-Dimensional
Organic Frameworks of 6-Mercaptonicotinic Acid: Unique Structural
Topologies Based on Selectivity for Hard and Soft Coordination Environments
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5981
_journal_page_last               5983
_journal_paper_doi               10.1021/ic050768q
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'C72 H50 Cs2 N12 Ni12 O32 S12, 8(H2 O)'
_chemical_formula_sum            'C72 H66 Cs2 N12 Ni12 O40 S12'
_chemical_formula_weight         3094.41
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           147
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_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                120.00
_cell_formula_units_Z            1
_cell_length_a                   19.0136(3)
_cell_length_b                   19.0136(3)
_cell_length_c                   8.5131(2)
_cell_measurement_reflns_used    28131
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      33.14
_cell_measurement_theta_min      1.02
_cell_volume                     2665.31(9)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
;
 HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_publication_material  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_solution    'SIR-92 (Altomare et al. 1994)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'Thin slice \w and \f scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_sigmaI/netI    0.0375
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            9498
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.71
_exptl_absorpt_coefficient_mu    3.061
_exptl_absorpt_correction_T_max  0.809
_exptl_absorpt_correction_T_min  0.659
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.922
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'hexagonal rod'
_exptl_crystal_F_000             1530
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.827
_refine_diff_density_min         -0.600
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         3107
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0299
_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^)+(0.0313P)^2^+4.3542P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0708
_refine_ls_wR_factor_ref         0.0720
_reflns_number_gt                2984
_reflns_number_total             3107
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050768qsi20050513_122735_2.cif
_cod_data_source_block           2
_cod_original_cell_volume        2665.30(9)
_cod_database_code               4309462