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_7042567
_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         'C56 H38 Er2, 2(C6 H6)'
_chemical_formula_sum            'C68 H50 Er2'
_chemical_formula_weight         1201.60
_chemical_name_systematic
;
 ?
;
_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             2015-02-12
_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                 96.756(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.6041(3)
_cell_length_b                   14.4756(7)
_cell_length_c                   15.4007(5)
_cell_measurement_reflns_used    13265
_cell_measurement_temperature    100.00(11)
_cell_measurement_theta_max      29.9590
_cell_measurement_theta_min      2.0790
_cell_volume                     2568.99(16)
_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      100.00(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0951
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9996
_diffrn_measured_fraction_theta_max 0.9937
_diffrn_measurement_details
;
  1 omega   -3.00   92.00   1.0000  122.0000
omega____ theta____ kappa____ phi______ frames
    -       24.9640   77.0000  120.0000 95

  2 omega    6.00   92.00   1.0000  122.0000
omega____ theta____ kappa____ phi______ frames
    -       24.9640   57.0000   60.0000 86

  3 omega    6.00   93.00   1.0000  122.0000
omega____ theta____ kappa____ phi______ frames
    -       24.9640   57.0000 -120.0000 87

  4 omega   -3.00   93.00   1.0000  122.0000
omega____ theta____ kappa____ phi______ frames
    -       24.9640   77.0000  -60.0000 96

  5 omega  -42.00   47.00   1.0000  122.0000
omega____ theta____ kappa____ phi______ frames
    -       24.9640  -38.0000   60.0000 89

  6 omega   35.00   83.00   1.0000  122.0000
omega____ theta____ kappa____ phi______ frames
    -       24.9640 -130.0000    3.1580 48

  7 omega   43.00   85.00   1.0000  122.0000
omega____ theta____ kappa____ phi______ frames
    -       24.9640 -133.0000  162.6617 42

  8 omega  -41.00   46.00   1.0000  122.0000
omega____ theta____ kappa____ phi______ frames
    -       24.9640  -38.0000 -120.0000 87

  9 omega  -46.00   47.00   1.0000  122.0000
omega____ theta____ kappa____ phi______ frames
    -       24.9640  -38.0000  -30.0000 93

 10 omega  -46.00   47.00   1.0000  122.0000
omega____ theta____ kappa____ phi______ frames
    -       24.9640  -38.0000  150.0000 93
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0090631000
_diffrn_orient_matrix_UB_12      -0.0336363000
_diffrn_orient_matrix_UB_13      -0.0319940000
_diffrn_orient_matrix_UB_21      -0.0563648000
_diffrn_orient_matrix_UB_22      0.0086724000
_diffrn_orient_matrix_UB_23      -0.0215793000
_diffrn_orient_matrix_UB_31      0.0229790000
_diffrn_orient_matrix_UB_32      0.0345850000
_diffrn_orient_matrix_UB_33      -0.0257088000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_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       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            49368
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.000
_diffrn_reflns_theta_min         1.937
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.286
_exptl_absorpt_correction_T_max  0.879
_exptl_absorpt_correction_T_min  0.791
_exptl_absorpt_correction_type   gaussian
_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)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1188
_exptl_crystal_size_max          0.1225
_exptl_crystal_size_mid          0.0682
_exptl_crystal_size_min          0.046
_refine_diff_density_max         4.063
_refine_diff_density_min         -1.795
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.385
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         7492
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.385
_refine_ls_R_factor_all          0.0939
_refine_ls_R_factor_gt           0.0763
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0023P)^2^+24.2725P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1469
_refine_ls_wR_factor_ref         0.1528
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5982
_reflns_number_total             7492
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00554g2.cif
_cod_data_source_block           compound12
_cod_depositor_comments
'Adding full bibliography for 7042559--7042570.cif.'
_cod_original_cell_volume        2568.99(17)
_cod_database_code               7042567
_chemical_oxdiff_formula         'C68 H50 Er2'
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_shelx_res_checksum              60713
_shelxl_version_number           2013-2