Macrocyclic Amines as Structure-Directing Agents for the Synthesis of Three-Dimensional Antimony-Sulfide Frameworks
Powell, Anthony V.; Lees, Rachel J. E.; Chippindale, Ann M.; Inorganic Chemistry 45 (2006) 4261–4267; doi:10.1021/ic060263f

data_4332344
_publ_section_title
;
 Macrocyclic Amines as Structure-Directing Agents for the Synthesis of
 Three-Dimensional Antimony-Sulfide Frameworks
;
_journal_issue                   10
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4261
_journal_page_last               4267
_journal_paper_doi               10.1021/ic060263f
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'S7 Sb4, C10 H24 N4 Ni'
_chemical_formula_sum            'C10 H24 N4 Ni S7 Sb4'
_chemical_formula_weight         970.55
_chemical_name_systematic        '[Ni(C10N4H24)][Sb4S7] compound 2'
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             05-06-08
_audit_creation_method           CRYSTALS_ver_12.50
_cell_angle_alpha                90
_cell_angle_beta                 102.772(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.7781(5)
_cell_length_b                   11.8694(5)
_cell_length_c                   15.3855(7)
_cell_measurement_reflns_used    3733
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.533
_cell_measurement_theta_min      2.485
_cell_volume                     2453.86(18)
_computing_cell_refinement       'APEX-2 (Bruker, 2005)'
_computing_data_collection       'APEX-2 (Bruker, 2005)'
_computing_data_reduction        'APEX-2 (Bruker, 2005)'
_computing_molecular_graphics    'ATOMS (Dowty, 2000)'
_computing_publication_material  'CRYSTALS (Watkin et al., 1996)'
_computing_structure_refinement  'CRYSTALS (Watkin et al., 1996)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
'Bruker -Nonius Apex-2 CCD area-detector diffractometer'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.052
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25506
_diffrn_reflns_theta_full        30.533
_diffrn_reflns_theta_max         30.533
_diffrn_reflns_theta_min         2.485
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.702
_exptl_absorpt_correction_T_max  0.6337
_exptl_absorpt_correction_T_min  0.4016
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS (Siemens, 1996)
;
_exptl_crystal_colour            'dark yellow'
_exptl_crystal_density_diffrn    2.627
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.95
_refine_diff_density_min         -1.19
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0634
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         1879
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0669
_refine_ls_R_factor_gt           0.0289
_refine_ls_shift/su_max          0.001551
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.842 0.547E-01 0.302 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0605
_refine_ls_wR_factor_gt          0.0324
_refine_ls_wR_factor_ref         0.0324
_reflns_limit_h_max              19
_reflns_limit_h_min              -19
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                1879
_reflns_number_total             3733
_reflns_threshold_expression     I>3.00u(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_scale          0.1305(2)
_oxford_structure_analysis_title 'X80466c2c in C2/c'
_cod_data_source_file            ic060263fsup2.cif
_cod_data_source_block           CRYSTALS_cif
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'multi scan'
changed to 'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'C 1 2/c 1 '
_cod_original_formula_sum        ' C10 H24 N4 Ni S7 Sb4'
_cod_database_code               4332344