Methylene-bridged, intramolecular donor-acceptor systems based on rare-earth metals and phosphinomethanides.
Pieper, Martin; Lamm, Jan-Hendrik; Neumann, Beate; Stammler, Hans-Georg; Mitzel, Norbert W.; Dalton transactions (Cambridge, England : 2003) 46 (2017) 5326–5336; doi:10.1039/c7dt00554g

data_7042562
_publ_section_title
;
 Methylene-bridged, intramolecular donor-acceptor systems based on
 rare-earth metals and phosphinomethanides.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5326
_journal_page_last               5336
_journal_paper_doi               10.1039/c7dt00554g
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C36 H30 Y2'
_chemical_formula_sum            'C36 H30 Y2'
_chemical_formula_weight         640.42
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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
_audit_creation_date             2017-02-09
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_audit_update_record
;
2017-02-10 deposited with the CCDC.
2017-03-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.2336(16)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.58646(13)
_cell_length_b                   10.33636(12)
_cell_length_c                   16.2330(3)
_cell_measurement_reflns_used    29064
_cell_measurement_temperature    99.9(2)
_cell_measurement_theta_max      72.0420
_cell_measurement_theta_min      4.2640
_cell_volume                     1417.80(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9996
_diffrn_measured_fraction_theta_max 0.9970
_diffrn_measurement_details
;
  1 omega -122.00  -35.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000 -178.0000 -180.0000 87

  2 omega   18.00  112.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   57.0000 -150.0000 94

  3 omega   18.00  112.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   57.0000  -60.0000 94

  4 omega  -28.00   64.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988  -38.0000  -30.0000 92

  5 omega   10.00   36.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   85.0000  177.8499 26

  6 omega   18.00  112.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   57.0000  -90.0000 94

  7 omega   18.00  112.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   57.0000   30.0000 94

  8 omega   13.00  115.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   77.0000  120.0000 102

  9 omega   13.00  115.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   77.0000    0.0000 102

 10 omega   23.00  114.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   38.0000    0.0000 91

 11 omega   13.00  115.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   77.0000   60.0000 102

 12 omega   57.00  127.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988  178.0000 -150.0000 70

 13 omega   13.00  115.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   77.0000  -90.0000 102

 14 omega  -25.00   68.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988  -57.0000  150.0000 93

 15 omega   81.00  178.00   1.0000    1.0800
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   30.0000 97

 16 omega   40.00  141.00   1.0000    1.0800
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -77.0000  -90.0000 101

 17 omega   85.00  178.00   1.0000    1.0800
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  150.0000 93

 18 omega   81.00  178.00   1.0000    1.0800
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -60.0000 97

 19 omega   85.00  178.00   1.0000    1.0800
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   30.0000 93

 20 omega   85.00  178.00   1.0000    1.0800
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  120.0000 93

 21 omega   81.00  178.00   1.0000    1.0800
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -30.0000 97

 22 omega   81.00  178.00   1.0000    1.0800
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   90.0000 97

 23 omega   85.00  178.00   1.0000    1.0800
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000 -120.0000 93

 24 omega   89.00  178.00   1.0000    1.0800
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000  150.0000 89

 25 omega   85.00  178.00   1.0000    1.0800
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000 -150.0000 93

 26 omega   81.00  178.00   1.0000    1.0800
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000   60.0000 97

 27 omega   81.00  178.00   1.0000    1.0800
omega____ theta____ kappa____ phi______ frames
    -      111.0000   75.0000   -5.4932 97

 28 omega   85.00  178.00   1.0000    1.0800
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   90.0000 93

 29 omega   81.00  178.00   1.0000    1.0800
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  150.0000 97

 30 omega   85.00  178.00   1.0000    1.0800
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000    0.0000 93

 31 omega   31.00  109.00   1.0000    1.0800
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000 -120.0000 78

 32 omega   81.00  178.00   1.0000    1.0800
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000    0.0000 97

 33 omega   81.00  178.00   1.0000    1.0800
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000 -150.0000 97

 34 omega   41.00  122.00   1.0000    1.0800
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000 -180.0000 81

 35 omega   31.00  109.00   1.0000    1.0800
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000 -180.0000 78

 36 omega   89.00  178.00   1.0000    1.0800
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000   60.0000 89

 37 omega   41.00  122.00   1.0000    1.0800
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000    0.0000 81

 38 omega   81.00  178.00   1.0000    1.0800
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  120.0000 97

 39 omega   85.00  178.00   1.0000    1.0800
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000 -180.0000 93

 40 omega   81.00  178.00   1.0000    1.0800
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000 -180.0000 97

 41 omega   85.00  178.00   1.0000    1.0800
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  -90.0000 93

 42 omega   85.00  178.00   1.0000    1.0800
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   60.0000 93

 43 omega   81.00  178.00   1.0000    1.0800
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -90.0000 97

 44 omega   85.00  178.00   1.0000    1.0800
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  -60.0000 93

 45 omega   81.00  178.00   1.0000    1.0800
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000 -120.0000 97

 46 omega   31.00  109.00   1.0000    1.0800
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000   60.0000 78

 47 omega   41.00   98.00   1.0000    1.0800
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000   30.0000 57

 48 omega   85.00  178.00   1.0000    1.0800
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  -26.7369 93

 49 omega   23.00  114.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   38.0000   90.0000 91

 50 omega   18.00  112.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   57.0000 -120.0000 94

 51 omega   18.00  112.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   57.0000  150.0000 94

 52 omega   13.00  115.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   77.0000   30.0000 102

 53 omega   13.00  115.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988   77.0000  -30.0000 102

 54 omega  -42.00  129.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988    0.0000 -180.0000 171

 55 omega  -42.00  129.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988    0.0000 -150.0000 171

 56 omega  -42.00  129.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988    0.0000 -120.0000 171

 57 omega  -42.00  129.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988    0.0000  -90.0000 171

 58 omega  -42.00  129.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988    0.0000  -60.0000 171

 59 omega  -42.00  129.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988    0.0000  -30.0000 171

 60 omega   57.00  127.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1988  178.0000 -180.0000 70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0246855000
_diffrn_orient_matrix_UB_12      0.1454621000
_diffrn_orient_matrix_UB_13      0.0186464000
_diffrn_orient_matrix_UB_21      -0.1692484000
_diffrn_orient_matrix_UB_22      0.0094703000
_diffrn_orient_matrix_UB_23      0.0188004000
_diffrn_orient_matrix_UB_31      0.0629354000
_diffrn_orient_matrix_UB_32      -0.0311053000
_diffrn_orient_matrix_UB_33      0.0927541000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0126
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            49565
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.349
_diffrn_reflns_theta_min         5.097
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.622
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72520
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_description       fragment
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.2468
_exptl_crystal_size_mid          0.1203
_exptl_crystal_size_min          0.0824
_refine_diff_density_max         0.608
_refine_diff_density_min         -0.730
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       0.00098(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/4 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         2810
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0294
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0333P)^2^+2.4743P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0731
_refine_ls_wR_factor_ref         0.0737
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2731
_reflns_number_total             2810
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00554g2.cif
_cod_data_source_block           compound7
_cod_depositor_comments
'Adding full bibliography for 7042559--7042570.cif.'
_cod_original_cell_volume        1417.81(4)
_cod_database_code               7042562
_chemical_oxdiff_formula         'C11 H10 N O'
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_date_sample_data_collection 2014-10-31
_olex2_date_sample_submission    4254591600
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9),
 C10(H10), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18)
;
_olex2_submission_special_instructions 'No special instructions were received'
_shelx_res_checksum              63043
_shelx_shelxl_version_number     2016/4