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_7050830
_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            'C17 H28 Cl2 N4 Ni O5'
_chemical_formula_weight         498.04
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.904(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.4121(8)
_cell_length_b                   9.0913(5)
_cell_length_c                   18.3528(12)
_cell_measurement_reflns_used    81
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.309
_cell_measurement_theta_min      5.547
_cell_volume                     2162.5(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.000
_diffrn_measured_fraction_theta_max 0.998
_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  0.0387
_diffrn_reflns_av_sigmaI/netI    0.0524
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7575
_diffrn_reflns_theta_full        0.50
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.10
_exptl_absorpt_coefficient_mu    1.180
_exptl_absorpt_correction_type   non
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.530
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.516
_refine_diff_density_min         -0.820
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.930
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         3794
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.930
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0742P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0965
_refine_ls_wR_factor_ref         0.1150
_reflns_number_gt                2736
_reflns_number_total             3794
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b200164k.txt
_cod_data_source_block           l1py
_cod_database_code               7050830