Complete stereocontrol in the synthesis of macrocyclic lanthanide complexes: direct formation of enantiopure systems for circularly polarised luminescence applications.
Evans, Nicholas H.; Carr, Rachel; Delbianco, Martina; Pal, Robert; Yufit, Dmitry S.; Parker, David; Dalton transactions (Cambridge, England : 2003) 42 (2013) 15610–15616; doi:10.1039/c3dt52425f

data_7023814
_publ_section_title
;
 Complete stereocontrol in the synthesis of macrocyclic lanthanide
 complexes: direct formation of enantiopure systems for circularly
 polarised luminescence applications.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15610
_journal_page_last               15616
_journal_paper_doi               10.1039/c3dt52425f
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C27 H33 Br3 Eu N6 O6 P3, 2(H2 O)'
_chemical_formula_sum            'C27 H37 Br3 Eu N6 O8 P3'
_chemical_formula_weight         1058.23
_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             2012-07-22
_audit_creation_method
;
  Olex2 1.2-beta
  (compiled 2012.05.09 svn.r2324, GUI svn.r4230)
;
_cell_angle_alpha                107.259(4)
_cell_angle_beta                 97.936(4)
_cell_angle_gamma                105.863(4)
_cell_formula_units_Z            2
_cell_length_a                   9.8356(4)
_cell_length_b                   12.3427(5)
_cell_length_c                   17.2609(8)
_cell_measurement_reflns_used    6712
_cell_measurement_temperature    120
_cell_measurement_theta_max      32.5660
_cell_measurement_theta_min      2.5559
_cell_volume                     1869.29(16)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.8 (release 13-04-2012 CrysAlis171 .NET)
(compiled Apr 13 2012,18:42:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.8 (release 13-04-2012 CrysAlis171 .NET)
(compiled Apr 13 2012,18:42:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.8 (release 13-04-2012 CrysAlis171 .NET)
(compiled Apr 13 2012,18:42:44)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      120
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 16.1511
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
  1 omega  -91.00    8.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.1867  -19.0000  -90.0000 99

  2 omega  -48.00   43.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.1867   57.0000   90.0000 91

  3 omega  -95.00   -5.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.1867  -57.0000 -150.0000 90

  4 omega    4.00   74.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9679 -108.0000  171.0000 70

  5 omega   73.00  103.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9679  179.0000   60.0000 30

  6 omega  -48.00  -23.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.1867   57.0000 -120.0000 25

  7 omega  -95.00   -5.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.1867  -57.0000   90.0000 90
;
_diffrn_measurement_device       '3-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       \w-scan
_diffrn_orient_matrix_UB_11      -0.0170463000
_diffrn_orient_matrix_UB_12      -0.0200041000
_diffrn_orient_matrix_UB_13      0.0331038000
_diffrn_orient_matrix_UB_21      0.0233082000
_diffrn_orient_matrix_UB_22      0.0605638000
_diffrn_orient_matrix_UB_23      0.0275949000
_diffrn_orient_matrix_UB_31      -0.0715955000
_diffrn_orient_matrix_UB_32      0.0016186000
_diffrn_orient_matrix_UB_33      -0.0102969000
_diffrn_radiation_collimation    monochromator
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_xray_symbol    Mo
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_av_unetI/netI     0.0703
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            21350
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.56
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_source_type              'sealed tube'
_exptl_absorpt_coefficient_mu    5.065
_exptl_absorpt_correction_T_max  0.723
_exptl_absorpt_correction_T_min  0.437
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.8 (release 13-04-2012 CrysAlis171 .NET)
(compiled Apr 13 2012,18:42:44)
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    1.880
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1036
_exptl_crystal_size_max          0.2852
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.0992
_refine_diff_density_max         1.760
_refine_diff_density_min         -1.014
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         10802
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0333P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0832
_refine_ls_wR_factor_ref         0.0918
_reflns_number_gt                8528
_reflns_number_total             10802
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt52425f.txt
_cod_data_source_block           12srv147
_cod_original_cell_volume        1869.30(14)
_cod_database_code               7023814
_reflns_odcompleteness_completeness 98.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44