Isostructural Series of Nine-Coordinate Chiral Lanthanide Complexes Based on Triazacyclononane
James W. Walton; Rachel Carr; Nicholas H. Evans; Alexander M. Funk; Alan M. Kenwright; David Parker; Dmitry S. Yufit; Mauro Botta; Sara De Pinto; Ka-Leung Wong; Inorganic Chemistry 51 (2012) 8042–8056; doi:10.1021/ic300147p

data_4329797
_publ_contact_author_address
;
Department of Chemistry
Durham University
South Rd., Durham
DH1 3LE, UK
;
_publ_contact_author_email       d.s.yufit@durham.ac.uk
_publ_contact_author_name        'Dmitry Yufit'
_publ_contact_author_phone       '+44 (0)191 3342004'
_publ_section_title
;
 Isostructural Series of Nine-Coordinate Chiral Lanthanide Complexes Based
 on Triazacyclononane
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8042
_journal_page_last               8056
_journal_paper_doi               10.1021/ic300147p
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C42 H42 Ce N6 O6 P3'
_chemical_formula_sum            'C42 H42 Ce N6 O6 P3'
_chemical_formula_weight         959.85
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-12-13
_audit_creation_method
;
  Olex2 1.1-beta
  (compiled 2011.11.01 svn.r2039, GUI svn.r3906)
;
_cell_angle_alpha                110.4195(19)
_cell_angle_beta                 99.5765(17)
_cell_angle_gamma                101.542(2)
_cell_formula_units_Z            2
_cell_length_a                   11.2660(2)
_cell_length_b                   14.0690(4)
_cell_length_c                   17.2816(3)
_cell_measurement_reflns_used    9562
_cell_measurement_temperature    120
_cell_measurement_theta_max      32.6296
_cell_measurement_theta_min      2.5619
_cell_volume                     2430.51(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_molecular_graphics
;
OLEX2
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
OLEX2
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 16.1511
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -90.00   -7.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.1867  -57.0000  -30.0000 166

  2 omega  -95.00  -33.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.1867  -57.0000  -60.0000 124

  3 omega  -49.00   41.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.1867   38.0000  120.0000 180

  4 omega -101.00  -76.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.1867 -179.0000  150.0000 50

  5 omega    2.00   87.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9679   38.0000 -150.0000 170

  6 omega   36.00   84.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9679 -133.0000  101.0000 96

  7 omega   70.00   97.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9679 -179.0000  -60.0000 54

  8 omega  -41.00   47.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9679  -57.0000 -150.0000 176

  9 omega  -33.00   -2.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9679  133.0000  170.0000 62

 10 omega -102.00  -58.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.1867 -179.0000 -120.0000 88

 11 omega  -95.00   -5.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.1867  -57.0000   60.0000 180
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0356140000
_diffrn_orient_matrix_UB_12      -0.0351920000
_diffrn_orient_matrix_UB_13      0.0036734000
_diffrn_orient_matrix_UB_21      -0.0555962000
_diffrn_orient_matrix_UB_22      -0.0425860000
_diffrn_orient_matrix_UB_23      -0.0175061000
_diffrn_orient_matrix_UB_31      0.0079000000
_diffrn_orient_matrix_UB_32      -0.0093222000
_diffrn_orient_matrix_UB_33      -0.0416411000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0545
_diffrn_reflns_av_unetI/netI     0.0742
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            40084
_diffrn_reflns_theta_full        29.50
_diffrn_reflns_theta_max         29.50
_diffrn_reflns_theta_min         2.57
_diffrn_source                   'Enhance (Mo) x-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    1.082
_exptl_absorpt_correction_T_max  0.949
_exptl_absorpt_correction_T_min  0.808
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_description       prism
_exptl_crystal_F_000             974
_exptl_crystal_size_max          0.286
_exptl_crystal_size_mid          0.1922
_exptl_crystal_size_min          0.0534
_refine_diff_density_max         0.769
_refine_diff_density_min         -0.709
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         13519
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0366
_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^)+(0.0390P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0801
_refine_ls_wR_factor_ref         0.0837
_reflns_number_gt                11247
_reflns_number_total             13519
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300147p_si_002.cif
_cod_data_source_block           CeL_11srv252
_cod_original_cell_volume        2430.50(9)
_cod_database_code               4329797
_chemical_oxdiff_formula         'C42 H42 N6 O6 P3 Ce1'
_reflns_odcompleteness_completeness 97.39
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.44