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_7702371
_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_structural     '[Ca(C18H18N4)2](ClO4)2'
_chemical_formula_sum            'C36 H36 Ca Cl2 N8 O8'
_chemical_formula_weight         819.715
_chemical_name_common
;
bis-tripicolylaminecalcium perchlorate
;
_chemical_name_systematic
;                                  
bis-tri(2-pyridylmethyl)aminecalcium diperchlorate                
;
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_type_scat_source           IntTabIV
_cell_angle_alpha                90.0
_cell_angle_beta                 103.411(1)
_cell_angle_gamma                90.0
_cell_formula_units_Z            2
_cell_length_a                   9.7069(5)
_cell_length_b                   10.8978(5)
_cell_length_c                   18.3622(9)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    120
_cell_measurement_theta_max      28.4
_cell_measurement_theta_min      2.2
_cell_volume                     1889.46(16)
_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  0.026
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12025
_diffrn_reflns_reduction_process 12025
_diffrn_reflns_theta_max         28.4
_diffrn_reflns_theta_min         2.2
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.370
_exptl_absorpt_correction_T_max  0.924
_exptl_absorpt_correction_T_min  0.871
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             852
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.34(5)
_refine_diff_density_min         -0.44(5)
_refine_ls_extinction_coef       110(26)
_refine_ls_extinction_method
;                                  
B-C type 1                         
Lorentzian isotropic (1974)
;
_refine_ls_goodness_of_fit_obs   1.757
_refine_ls_hydrogen_treatment    constraint
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     251
_refine_ls_number_reflns         3903
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.029
_refine_ls_shift/esd_max         0.00093
_refine_ls_shift/esd_mean        0.00007
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/{[\s~cs~(F^2^)+1.03F^2^]^1/2^-|F|}^2^'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.051
_reflns_number_observed          3903
_reflns_number_total             4561
_reflns_observed_criterion       I>3\s(I)
_cod_data_source_file            900359b.txt
_cod_data_source_block           jgm2
_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^)+1.03F^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^)+1.03F^2^]^1/2^-|F|}^2^'.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        1889.5(1)
_cod_original_sg_symbol_H-M      '1 P21/n 1'
_cod_original_formula_sum        C36H36N8O8Cl2Ca
_cod_database_code               7702371