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_7011161
_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            'C19 H30 Cl N3 O'
_chemical_formula_weight         351.91
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 102.868(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.5465(4)
_cell_length_b                   12.7121(7)
_cell_length_c                   14.9812(6)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.96
_cell_measurement_theta_min      11.13
_cell_volume                     1958.06(16)
_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      293(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  0.0311
_diffrn_reflns_av_sigmaI/netI    0.0317
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            3299
_diffrn_reflns_theta_max         62.98
_diffrn_reflns_theta_min         4.61
_diffrn_standards_decay_%        2.37
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.796
_exptl_absorpt_correction_T_max  0.8425
_exptl_absorpt_correction_T_min  0.5038
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Clear
_exptl_crystal_density_diffrn    1.194
_exptl_crystal_description       'Prismatic needles'
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.93
_exptl_crystal_size_mid          0.57
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.260
_refine_diff_density_min         -0.266
_refine_diff_density_rms         0.029
_refine_ls_extinction_coef       0.0092(14)
_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   1.040
_refine_ls_goodness_of_fit_obs   1.084
_refine_ls_matrix_type           full
_refine_ls_number_parameters     234
_refine_ls_number_reflns         2938
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.061
_refine_ls_restrained_S_obs      1.086
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_obs          0.0457
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0507P)^2^+0.5968P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1203
_refine_ls_wR_factor_obs         0.1106
_reflns_number_observed          2548
_reflns_number_total             3116
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b108235n.txt
_cod_data_source_block           NL9703
_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.

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' 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^)+(0.0507P)^2^+0.5968P] 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^)+(0.0507P)^2^+0.5968P] 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        1958.1(2)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7011161