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_7042561
_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 Y2, 3(C7 H8)(squeezed)'
_chemical_formula_sum            'C77 H62 Y2'
_chemical_formula_weight         1165.08
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2yc'
_space_group_name_H-M_alt        'I 1 2/c 1'
_symmetry_space_group_name_Hall  '-I 2yc'
_symmetry_space_group_name_H-M   'I 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-05-07
_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                 103.266(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.6353(3)
_cell_length_b                   22.9872(5)
_cell_length_c                   19.9472(4)
_cell_measurement_reflns_used    16120
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      72.0330
_cell_measurement_theta_min      2.9480
_cell_volume                     5639.1(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.30a (Agilent, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.30a (Agilent, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.30a (Agilent, 2015)'
_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    'J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_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 0.9967
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -63.00  30.00   1.00   11.00    --  -38.50  57.00  30.00   93
  2  \w    -96.00 -18.00   1.00   11.00    --  -38.50 -38.00  90.00   78
  3  \w    -64.00  30.00   1.00   11.00    --  -38.50  57.00 -90.00   94
  4  \w   -107.00 -39.00   1.00   11.00    --  -38.50 -77.00-120.00   68
  5  \w    -64.00  30.00   1.00   11.00    --  -38.50  57.00 150.00   94
  6  \w    -33.00  -8.00   1.00   11.00    --  -38.50 -77.00-120.00   25
  7  \w     81.00 107.00   1.00   11.00    --   42.95  57.00-150.00   26
  8  \w     14.00  78.00   1.00   11.00    --   42.95  77.00 -60.00   64
  9  \w     14.00 111.00   1.00   11.00    --   42.95  77.00   0.00   97
 10  \w     64.00 106.00   1.00   11.00    --   42.95  57.00 -90.00   42
 11  \w     18.00  78.00   1.00   11.00    --   42.95  57.00-150.00   60
 12  \w     11.00  38.00   1.00   11.00    --   42.95  84.00 171.51   27
 13  \w     30.00  82.00   1.00   11.00    --   42.95 -99.00-120.00   52
 14  \w     87.00 114.00   1.00   11.00    --   42.95  77.00 -60.00   27
 15  \w     13.00  70.00   1.00   11.00    --   42.95  77.00  90.00   57
 16  \w     82.00 120.00   1.00   11.00    --   42.95 178.00 150.00   38
 17  \w     19.00  58.00   1.00   11.00    --   42.95  57.00 -90.00   39
 18  \w     53.00  92.00   1.00   49.50    --  111.00 -94.00  60.00   39
 19  \w    118.00 176.00   1.00   49.50    --  111.00  77.00  60.00   58
 20  \w     82.00 128.00   1.00   49.50    --  111.00  72.00  89.84   46
 21  \w     84.00 109.00   1.00   49.50    --  111.00 -94.00-120.00   25
 22  \w     81.00 147.00   1.00   49.50    --  111.00  77.00-120.00   66
 23  \w     81.00 178.00   1.00   49.50    --  111.00  77.00 -60.00   97
 24  \w     46.00  73.00   1.00   49.50    --  111.00 -94.00-120.00   27
 25  \w     45.00 133.00   1.00   49.50    --  111.00 -61.00 -90.00   88
 26  \w     81.00 107.00   1.00   49.50    --  111.00  77.00  60.00   26
 27  \w     89.00 151.00   1.00   49.50    --  111.00  45.00   0.00   62
 28  \w     81.00 107.00   1.00   49.50    --  111.00  77.00 -30.00   26
 29  \w     82.00 107.00   1.00   49.50    --  111.00  77.00-150.00   25
 30  \w    115.00 178.00   1.00   49.50    --  111.00  77.00-150.00   63
 31  \w     83.00 109.00   1.00   49.50    --  111.00  67.00 124.63   26
 32  \w     85.00 110.00   1.00   49.50    --  111.00  65.00 -56.62   25
 33  \w     85.00 128.00   1.00   49.50    --  111.00  61.00-150.00   43
 34  \w     85.00 177.00   1.00   49.50    --  111.00  61.00   0.00   92
 35  \w     81.00 108.00   1.00   49.50    --  111.00  76.00 -98.89   27
 36  \w     96.00 141.00   1.00   49.50    --  111.00 -77.00 150.00   45
 37  \w     81.00 108.00   1.00   49.50    --  111.00  77.00  30.00   27
 38  \w     42.00 122.00   1.00   49.50    --  111.00-125.00-120.00   80
 39  \w     42.00  69.00   1.00   49.50    --  111.00 -77.00 150.00   27
 40  \w     82.00 108.00   1.00   49.50    --  111.00  72.00 135.48   26
 41  \w    111.00 178.00   1.00   49.50    --  111.00  77.00  30.00   67
 42  \w     85.00 112.00   1.00   49.50    --  111.00  61.00  60.00   27
 43  \w     85.00 114.00   1.00   49.50    --  111.00  65.00  33.41   29
 44  \w     85.00 111.00   1.00   49.50    --  111.00  61.00-180.00   26
 45  \w     85.00 112.00   1.00   49.50    --  111.00  61.00 -60.00   27
 46  \w     85.00 126.00   1.00   49.50    --  111.00  61.00 -90.00   41
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0999627000
_diffrn_orient_matrix_UB_12      -0.0051147000
_diffrn_orient_matrix_UB_13      0.0316405000
_diffrn_orient_matrix_UB_21      0.0755593000
_diffrn_orient_matrix_UB_22      -0.0065316000
_diffrn_orient_matrix_UB_23      0.0721356000
_diffrn_orient_matrix_UB_31      -0.0003087000
_diffrn_orient_matrix_UB_32      0.0664927000
_diffrn_orient_matrix_UB_33      0.0094945000
_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  0.0350
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            37883
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.28
_diffrn_reflns_theta_min         2.98
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.090
_exptl_absorpt_correction_T_max  0.972
_exptl_absorpt_correction_T_min  0.943
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.30a (Agilent, 2015)
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    1.372
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2408
_exptl_crystal_size_max          0.124
_exptl_crystal_size_mid          0.089
_exptl_crystal_size_min          0.039
_refine_diff_density_max         0.778
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         5544
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0334
_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^)+(0.0499P)^2^+5.4927P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0909
_refine_ls_wR_factor_ref         0.0936
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4618
_reflns_number_total             5544
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00554g2.cif
_cod_data_source_block           compound10
_cod_depositor_comments
'Adding full bibliography for 7042559--7042570.cif.'
_cod_database_code               7042561
_chemical_oxdiff_formula         'C69 H52 Y2'
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.191
_oxdiff_exptl_absorpt_empirical_full_min 0.841
_shelx_res_checksum              79406
_shelxl_version_number           2014-3