Conformational analysis of complexes of 2,4,4-trimethyl-1,5,9-triazacyclododec-1-ene and its 9-methyl derivative
Pérez, José; García, Luis; Guy Orpen, A.; Dolores Santana, M.; Saez, Paloma; García, Gabriel; New Journal of Chemistry 26 (2002) 726–; doi:10.1039/b200164k

data_7050831
_publ_section_title
;
 Conformational analysis of complexes of
 2,4,4-trimethyl-1,5,9-triazacyclododec-1-ene and its 9-methyl
 derivative
;
_journal_issue                   6
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              726
_journal_paper_doi               10.1039/b200164k
_journal_volume                  26
_journal_year                    2002
_chemical_formula_sum            'C19 H33 F6 N4 Ni O P'
_chemical_formula_weight         537.17
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                108.628(7)
_cell_angle_beta                 95.446(7)
_cell_angle_gamma                97.430(6)
_cell_formula_units_Z            2
_cell_length_a                   9.2990(9)
_cell_length_b                   10.5724(10)
_cell_length_c                   12.8248(13)
_cell_measurement_reflns_used    64
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      12.307
_cell_measurement_theta_min      4.791
_cell_volume                     1172.2(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.000
_diffrn_measured_fraction_theta_max 0.978
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0500
_diffrn_reflns_av_sigmaI/netI    0.0731
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4263
_diffrn_reflns_theta_full        0.50
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    0.962
_exptl_absorpt_correction_T_max  0.900
_exptl_absorpt_correction_T_min  0.742
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.190
_refine_diff_density_min         -0.985
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.205
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         4023
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.205
_refine_ls_R_factor_all          0.1162
_refine_ls_R_factor_gt           0.0740
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1375P)^2^+0.4896P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2001
_refine_ls_wR_factor_ref         0.2570
_reflns_number_gt                2661
_reflns_number_total             4023
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b200164k.txt
_cod_data_source_block           6me1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7050831