Synthesis, characterisation and polymerisation of vinylbenzene-substituted triazacyclododecanes and their transition metal complexes
Long, Nicholas J.; Parker, David G.; Speyer, Paul R.; White, Andrew J. P.; Williams, David J.; Journal of the Chemical Society, Dalton Transactions  (2002) 2142–; doi:10.1039/b108235n

data_7011162
_publ_section_title
;
 Synthesis, characterisation and polymerisation of
 vinylbenzene-substituted triazacyclododecanes and their transition
 metal complexes
;
_journal_issue                   10
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2142
_journal_paper_doi               10.1039/b108235n
_journal_year                    2002
_chemical_formula_sum            'C38.75 H61.5 Cl9.5 N6 Ni2 O'
_chemical_formula_weight         1081.63
_chemical_name_systematic
; 
? 
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 92.750(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   18.8284(13)
_cell_length_b                   28.2797(14)
_cell_length_c                   38.356(3)
_cell_measurement_reflns_used    36
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.51
_cell_measurement_theta_min      10.69
_cell_volume                     20400(2)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0854
_diffrn_reflns_av_sigmaI/netI    0.0779
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            15672
_diffrn_reflns_theta_max         60.01
_diffrn_reflns_theta_min         2.31
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.778
_exptl_absorpt_correction_T_max  0.2163
_exptl_absorpt_correction_T_min  0.0936
_exptl_absorpt_correction_type   Ellipsoidal
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_description       prisms
_exptl_crystal_F_000             8984
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.799
_refine_diff_density_min         -0.891
_refine_diff_density_rms         0.116
_refine_ls_extinction_coef       0.000015(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.045
_refine_ls_goodness_of_fit_obs   1.107
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1102
_refine_ls_number_reflns         13792
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.108
_refine_ls_restrained_S_obs      1.110
_refine_ls_R_factor_all          0.1265
_refine_ls_R_factor_obs          0.0875
_refine_ls_shift/esd_max         -0.060
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1413P)^2^+84.1615P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2692
_refine_ls_wR_factor_obs         0.2239
_reflns_number_observed          10581
_reflns_number_total             15145
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b108235n.txt
_cod_data_source_block           NL9801
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1413P)^2^+84.1615P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1413P)^2^+84.1615P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        20399.6(24)
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C38.75 H61.50 Cl9.50 N6 Ni2 O'
_cod_database_code               7011162