Synthesis and structural characterisation of Group I and II metal complexes involving the ligand tris(2-pyridylmethyl)amine
Hazell, Alan; McGinley, John; Toftlund, Hans; Journal of the Chemical Society, Dalton Transactions  (1999) 1271–; doi:10.1039/a900359b

data_7702370
_publ_section_title
;
 Synthesis and structural characterisation of Group I and II metal
 complexes involving the ligand tris(2-pyridylmethyl)amine
;
_journal_issue                   8
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1271
_journal_paper_doi               10.1039/a900359b
_journal_year                    1999
_chemical_formula_moiety         '[N(CH2C5H5N)3](SO4)(NO3)'
_chemical_formula_sum            'C18 H21 N5 O7 S'
_chemical_formula_weight         451.45
_chemical_name_common            'tripicolinium nitrate sulphate'
_chemical_name_systematic
;                                  
tris-2-methylpiridinium nitrate sulphate 
;
_space_group_IT_number           198
_space_group_name_Hall           'P 2ac 2ab 3'
_space_group_name_H-M_alt        'P 21 3'
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P 21 3'
_atom_type_scat_source           IntTabIV
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.6301(4)
_cell_length_b                   12.6301(4)
_cell_length_c                   12.6301(4)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    120
_cell_measurement_theta_max      26.9
_cell_measurement_theta_min      2.3
_cell_volume                     2014.75(11)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_molecular_graphics
;                                  
      ORTEP-III (Burnett & Johnson, 1996), KRYSTAL                    
;
_computing_publication_material  KRYSTAL
_computing_structure_refinement  'modified ORFLS(1962), KRYSTAL'
_computing_structure_solution
;                                  
     SIR97 (Cascarano et al., 1996) KRYSTAL                           
;
_diffrn_ambient_temperature      120
_diffrn_measurement_device       'Siemens SMART CCD diffractometer'
_diffrn_measurement_method       '\w rotation scans with narrow frames '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'x-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.037
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11037
_diffrn_reflns_reduction_process 11037
_diffrn_reflns_theta_max         26.9
_diffrn_reflns_theta_min         2.3
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.214
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_correction_T_min  0.920
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.66(8)
_refine_diff_density_min         -0.48(8)
_refine_ls_abs_structure_details
;                                  
refine Rogers factor for S         
;
_refine_ls_abs_structure_Rogers  -0.80(19)
_refine_ls_extinction_coef       278(66)
_refine_ls_extinction_method
;                                  
B-C type 1                         
Lorentzian isotropic (1974)
;
_refine_ls_goodness_of_fit_obs   3.640
_refine_ls_hydrogen_treatment    refine_xyzUiso
_refine_ls_matrix_type           full
_refine_ls_number_constraints    24
_refine_ls_number_parameters     124
_refine_ls_number_reflns         1346
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.035
_refine_ls_shift/esd_max         0.0011
_refine_ls_shift/esd_mean        0.0002
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/{[\s~cs~(F^2^)+1.01F^2^]^1/2^-|F|}^2^'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.050
_reflns_number_observed          1346
_reflns_number_total             1382
_reflns_observed_criterion       I>3\s(I)
_cod_data_source_file            900359b.txt
_cod_data_source_block           jgm1
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

data item '_refine_ls_weighting_scheme' value '
1/{[\s~cs~(F^2^)+1.01F^2^]^1/2^-|F|}^2^ ' was changed to 'calc'. A
new data item '_refine_ls_weighting_details' was created with the
value set to 'w = 1/{[\s~cs~(F^2^)+1.01F^2^]^1/2^-|F|}^2^'.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        2014.8(1)
_cod_original_sg_symbol_H-M      P213
_cod_original_formula_sum        C18H21N5O7S
_cod_database_code               7702370