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_7042565
_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         'C34 H52 Ho2 P2'
_chemical_formula_sum            'C34 H52 Ho2 P2'
_chemical_formula_weight         852.55
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-07-23
_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                 107.146(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.9053(5)
_cell_length_b                   8.6474(2)
_cell_length_c                   22.3820(5)
_cell_measurement_reflns_used    12877
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      71.9300
_cell_measurement_theta_min      4.1130
_cell_volume                     3311.48(15)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_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(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9984
_diffrn_measured_fraction_theta_max 0.9940
_diffrn_measurement_details
;
  1 omega -122.00  -35.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000 -178.0000  -60.0000 87

  2 omega  -48.00   24.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000    0.0000 72

  3 omega -106.00  -80.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -57.0000 -150.0000 26

  4 omega  -39.00  -14.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -57.0000 -150.0000 25

  5 omega   66.00   95.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000 -120.0000 29

  6 omega   13.00   46.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   81.0000  -79.9841 33

  7 omega   19.00  108.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   19.0000  -30.0000 89

  8 omega   58.00  120.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488  178.0000 -150.0000 62

  9 omega   13.00   93.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000  120.0000 80

 10 omega   14.00   63.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000   60.0000 49

 11 omega   87.00  114.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   38.0000   60.0000 27

 12 omega   65.00   93.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488  178.0000  -60.0000 28

 13 omega   14.00   77.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000    0.0000 63

 14 omega   18.00   53.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   57.0000  -30.0000 35

 15 omega   59.00  112.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   57.0000  -30.0000 53

 16 omega   14.00   59.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000 -120.0000 45

 17 omega   83.00  115.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000   60.0000 32

 18 omega   81.00  111.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000    0.0000 30

 19 omega   13.00  113.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   77.0000 -180.0000 100

 20 omega   57.00  125.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488  178.0000  -30.0000 68

 21 omega   25.00   62.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4488   38.0000   60.0000 37

 22 omega   85.00  111.00   1.0000   47.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  -60.0000 26

 23 omega   40.00  139.00   1.0000   47.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -77.0000  -90.0000 99

 24 omega   84.00  110.00   1.0000   47.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   64.0000 -141.5185 26

 25 omega   85.00  177.00   1.0000   47.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   30.0000 92

 26 omega   52.00   79.00   1.0000   47.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000 -180.0000 27

 27 omega   81.00  106.00   1.0000   47.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -60.0000 25

 28 omega  130.00  178.00   1.0000   47.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  -60.0000 48

 29 omega   85.00  111.00   1.0000   47.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000   90.0000 26

 30 omega   81.00  134.00   1.0000   47.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000 -120.0000 53

 31 omega   85.00  111.00   1.0000   47.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000 -150.0000 26

 32 omega   85.00  118.00   1.0000   47.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000 -180.0000 33

 33 omega   81.00  108.00   1.0000   47.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   76.0000  -98.1069 27

 34 omega   86.00  111.00   1.0000   47.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   59.0000  129.1805 25

 35 omega   83.00  177.00   1.0000   47.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   68.0000  -80.6316 94

 36 omega   85.00  111.00   1.0000   47.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  150.0000 26

 37 omega   85.00  111.00   1.0000   47.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  120.0000 26

 38 omega   82.00  108.00   1.0000   47.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   71.0000   -0.7690 26

 39 omega  117.00  178.00   1.0000   47.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  120.0000 61

 40 omega   81.00  109.00   1.0000   47.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  120.0000 28

 41 omega   33.00   95.00   1.0000   47.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000 -120.0000 62

 42 omega   85.00  164.00   1.0000   47.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  -90.0000 79

 43 omega  111.00  177.00   1.0000   47.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000 -150.0000 66

 44 omega   66.00  122.00   1.0000   47.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000   90.0000 56

 45 omega   54.00   80.00   1.0000   47.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -123.0000  -44.0000 26

 46 omega   92.00  120.00   1.0000   47.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -123.0000  -44.0000 28

 47 omega   84.00  162.00   1.0000   47.5000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   63.0000   -3.6674 78
;
_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      -0.0270434000
_diffrn_orient_matrix_UB_12      -0.0213446000
_diffrn_orient_matrix_UB_13      -0.0715011000
_diffrn_orient_matrix_UB_21      0.0671314000
_diffrn_orient_matrix_UB_22      -0.1156585000
_diffrn_orient_matrix_UB_23      0.0051752000
_diffrn_orient_matrix_UB_31      -0.0535536000
_diffrn_orient_matrix_UB_32      -0.1339006000
_diffrn_orient_matrix_UB_33      0.0068802000
_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  0.0343
_diffrn_reflns_av_unetI/netI     0.0174
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            21205
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.991
_diffrn_reflns_theta_min         4.134
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.694
_exptl_absorpt_correction_T_max  0.638
_exptl_absorpt_correction_T_min  0.422
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.710
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.1289
_exptl_crystal_size_mid          0.0647
_exptl_crystal_size_min          0.0624
_refine_diff_density_max         1.429
_refine_diff_density_min         -0.702
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         3258
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0273
_refine_ls_R_factor_gt           0.0258
_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^)+(0.0261P)^2^+11.3513P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0627
_refine_ls_wR_factor_ref         0.0638
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3099
_reflns_number_total             3258
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00554g2.cif
_cod_data_source_block           compound2
_cod_depositor_comments
'Adding full bibliography for 7042559--7042570.cif.'
_cod_original_cell_volume        3311.47(15)
_cod_database_code               7042565
_chemical_oxdiff_formula         C34H52P2Ho2
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'
_shelx_res_checksum              88166
_shelxl_version_number           2014-3