#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:59:31 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179946 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/41/7024150.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7024150
loop_
_publ_author_name
'Wooles, Ashley J.'
'Mills, David P.'
'Lewis, William'
'Blake, Alexander J.'
'Liddle, Stephen T.'
_publ_section_title
;
 Lanthanide tri-benzyl complexes: structural variations and useful
 precursors to phosphorus-stabilised lanthanide carbenes.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              500
_journal_page_last               510
_journal_paper_doi               10.1039/b911717b
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C42 H53 Er N2 O P2 Si2'
_chemical_formula_sum            'C42 H53 Er N2 O P2 Si2'
_chemical_formula_weight         887.24
_chemical_name_systematic
;
?
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   'geom, Me from difmap'
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           'enCIFer editing of SHELXL97 CIF output'
_cell_angle_alpha                90.00
_cell_angle_beta                 93.416(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.4181(4)
_cell_length_b                   19.2561(8)
_cell_length_c                   10.6622(4)
_cell_measurement_reflns_used    3496
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.65
_cell_measurement_theta_min      2.22
_cell_volume                     2135.16(15)
_computing_cell_refinement       'Bruker SAINT version 6.36A (Bruker, 2000)'
_computing_data_collection       'Bruker SMART version 5.625 (Bruker, 2001)'
_computing_data_reduction        'Bruker SAINT; SHELXTL (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material
'enCIFer (Allen et al., 2004); PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.544
_diffrn_measured_fraction_theta_max 0.544
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0216
_diffrn_reflns_av_sigmaI/netI    0.0451
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5626
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.96
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.129
_exptl_absorpt_correction_T_max  0.72
_exptl_absorpt_correction_T_min  0.54
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             906
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.429
_refine_diff_density_min         -0.320
_refine_diff_density_rms         0.050
_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     268
_refine_ls_number_reflns         2117
_refine_ls_number_restraints     180
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0186
_refine_ls_R_factor_gt           0.0183
_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/[σ²(Fo²)+(0.0000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0468
_refine_ls_wR_factor_ref         0.0469
_reflns_number_gt                2074
_reflns_number_total             2117
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b911717b.txt
_cod_data_source_block           19
_cod_original_cell_volume        2135.16(14)
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               7024150
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Er1 Er 0.727141(18) 0.7500 0.601443(18) 0.02033(8) Uani 1 2 d S . .
C1 C 0.8141(4) 0.7500 0.8088(4) 0.0212(9) Uani 1 2 d S . .
P1 P 0.85723(7) 0.83254(3) 0.79801(8) 0.01948(17) Uani 1 1 d . . .
C2 C 0.7895(3) 0.88322(13) 0.9225(3) 0.0216(6) Uani 1 1 d . A .
C3 C 0.8491(3) 0.93863(14) 0.9821(3) 0.0319(8) Uani 1 1 d . . .
H3 H 0.9325 0.9519 0.9598 0.038 Uiso 1 1 calc R A .
C4 C 0.7897(4) 0.97607(17) 1.0750(4) 0.0380(9) Uani 1 1 d . A .
H4 H 0.8339 1.0129 1.1182 0.046 Uiso 1 1 calc R . .
C5 C 0.6658(3) 0.95880(17) 1.1033(4) 0.0358(8) Uani 1 1 d . . .
H5 H 0.6230 0.9852 1.1635 0.043 Uiso 1 1 calc R A .
C6 C 0.6040(3) 0.90319(17) 1.0440(3) 0.0360(8) Uani 1 1 d . A .
H6 H 0.5194 0.8911 1.0644 0.043 Uiso 1 1 calc R . .
C7 C 0.6650(3) 0.86530(15) 0.9553(4) 0.0313(8) Uani 1 1 d . . .
H7 H 0.6225 0.8267 0.9161 0.038 Uiso 1 1 calc R A .
C8 C 1.0307(3) 0.84744(13) 0.8164(3) 0.0243(7) Uani 1 1 d . A .
C9 C 1.0980(3) 0.86041(16) 0.7106(4) 0.0326(8) Uani 1 1 d . . .
H9 H 1.0528 0.8664 0.6314 0.039 Uiso 1 1 calc R A .
C10 C 1.2321(3) 0.86467(18) 0.7201(4) 0.0411(10) Uani 1 1 d . A .
H10 H 1.2780 0.8734 0.6474 0.049 Uiso 1 1 calc R . .
C11 C 1.2972(3) 0.85618(17) 0.8350(4) 0.0421(10) Uani 1 1 d . . .
H11 H 1.3884 0.8587 0.8415 0.050 Uiso 1 1 calc R A .
C12 C 1.2310(4) 0.84409(17) 0.9406(5) 0.0428(10) Uani 1 1 d . A .
H12 H 1.2761 0.8394 1.0202 0.051 Uiso 1 1 calc R . .
C13 C 1.0960(3) 0.83878(15) 0.9301(4) 0.0341(9) Uani 1 1 d . . .
H13 H 1.0502 0.8291 1.0025 0.041 Uiso 1 1 calc R A .
N1 N 0.8010(2) 0.85994(11) 0.6617(2) 0.0205(5) Uani 1 1 d . A .
Si1 Si 0.76089(9) 0.94218(4) 0.60972(9) 0.0253(2) Uani 1 1 d . . .
C14 C 0.6059(3) 0.97245(16) 0.6702(4) 0.0404(9) Uani 1 1 d . A .
H14A H 0.5389 0.9377 0.6508 0.061 Uiso 1 1 calc R . .
H14B H 0.5810 1.0167 0.6303 0.061 Uiso 1 1 calc R . .
H14C H 0.6166 0.9789 0.7615 0.061 Uiso 1 1 calc R . .
C15 C 0.8859(4) 1.00963(15) 0.6551(4) 0.0441(10) Uani 1 1 d . A .
H15A H 0.8853 1.0189 0.7455 0.066 Uiso 1 1 calc R . .
H15B H 0.8667 1.0526 0.6083 0.066 Uiso 1 1 calc R . .
H15C H 0.9710 0.9925 0.6352 0.066 Uiso 1 1 calc R . .
C16 C 0.7415(4) 0.93790(18) 0.4345(4) 0.0420(9) Uani 1 1 d . A .
H16A H 0.8199 0.9187 0.4015 0.063 Uiso 1 1 calc R . .
H16B H 0.7264 0.9847 0.4007 0.063 Uiso 1 1 calc R . .
H16C H 0.6682 0.9080 0.4096 0.063 Uiso 1 1 calc R . .
C17 C 0.5013(4) 0.7500 0.6237(5) 0.0388(12) Uani 1 2 d S A .
H17A H 0.4735 0.7080 0.6684 0.047 Uiso 0.50 1 calc PR . .
H17B H 0.4735 0.7920 0.6684 0.047 Uiso 0.50 1 calc PR . .
C18 C 0.4535(5) 0.7500 0.4939(5) 0.0359(11) Uani 1 2 d S . .
C19 C 0.4337(4) 0.81177(17) 0.4242(4) 0.0444(9) Uani 1 1 d . A .
H19 H 0.4459 0.8551 0.4658 0.053 Uiso 1 1 calc R . .
C20 C 0.3975(6) 0.81137(19) 0.2986(4) 0.0682(15) Uani 1 1 d . . .
H20 H 0.3827 0.8541 0.2557 0.082 Uiso 1 1 calc R A .
C21 C 0.3822(9) 0.7500 0.2338(6) 0.085(3) Uani 1 2 d S . .
H21 H 0.3615 0.7500 0.1458 0.102 Uiso 1 2 calc SR . .
O1 O 0.8139(3) 0.7500 0.4039(3) 0.0386(8) Uani 0.50 2 d SPDU A 1
C22 C 0.7521(5) 0.7500 0.2798(4) 0.0448(11) Uani 0.50 2 d SPDU A 1
H22C H 0.6828 0.7852 0.2727 0.054 Uiso 0.25 1 calc PR A 1
H22D H 0.7149 0.7038 0.2589 0.054 Uiso 0.25 1 calc PR A 1
C23 C 0.8576(19) 0.768(2) 0.195(2) 0.049(2) Uani 0.25 1 d PDU A 1
H23C H 0.8654 0.8185 0.1847 0.058 Uiso 0.25 1 calc PR A 1
H23D H 0.8404 0.7464 0.1107 0.058 Uiso 0.25 1 calc PR A 1
C24 C 0.979(2) 0.7374(18) 0.2595(10) 0.055(3) Uani 0.25 1 d PDU A 1
H24C H 1.0573 0.7627 0.2361 0.067 Uiso 0.25 1 calc PR A 1
H24D H 0.9890 0.6874 0.2410 0.067 Uiso 0.25 1 calc PR A 1
C25 C 0.9511(4) 0.7500 0.3963(5) 0.0590(13) Uani 0.50 2 d SPDU A 1
H25C H 0.9903 0.7129 0.4503 0.071 Uiso 0.25 1 calc PR A 1
H25D H 0.9873 0.7952 0.4251 0.071 Uiso 0.25 1 calc PR A 1
O1A O 0.8139(3) 0.7500 0.4039(3) 0.0386(8) Uani 0.50 2 d SPDU A 2
C22A C 0.7521(5) 0.7500 0.2798(4) 0.0448(11) Uani 0.50 2 d SPDU A 2
H22A H 0.7074 0.7948 0.2634 0.054 Uiso 0.25 1 calc PR A 2
H22B H 0.6877 0.7122 0.2719 0.054 Uiso 0.25 1 calc PR A 2
C23A C 0.8536(19) 0.739(3) 0.187(2) 0.050(3) Uani 0.25 1 d PDU A 2
H23A H 0.8314 0.7623 0.1053 0.060 Uiso 0.25 1 calc PR A 2
H23B H 0.8727 0.6897 0.1735 0.060 Uiso 0.25 1 calc PR A 2
C24A C 0.962(3) 0.7765(15) 0.2623(12) 0.055(3) Uani 0.25 1 d PDU A 2
H24A H 0.9503 0.8275 0.2582 0.066 Uiso 0.25 1 calc PR A 2
H24B H 1.0465 0.7645 0.2307 0.066 Uiso 0.25 1 calc PR A 2
C25A C 0.9511(4) 0.7500 0.3963(5) 0.0590(13) Uani 0.50 2 d SPDU A 2
H25A H 0.9876 0.7028 0.4073 0.071 Uiso 0.25 1 calc PR A 2
H25B H 0.9937 0.7817 0.4589 0.071 Uiso 0.25 1 calc PR A 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N1 Er1 N1 130.66(12) . 4_575
N1 Er1 C1 68.68(7) . .
N1 Er1 C1 68.68(7) 4_575 .
N1 Er1 O1 96.27(7) . .
N1 Er1 O1 96.27(7) 4_575 .
C1 Er1 O1 134.60(12) . .
N1 Er1 C17 106.55(8) . .
N1 Er1 C17 106.55(8) 4_575 .
C1 Er1 C17 103.61(17) . .
O1 Er1 C17 121.80(15) . .
P1 C1 P1 147.0(3) . 4_575
P1 C1 Er1 91.45(16) . .
P1 C1 Er1 91.45(16) 4_575 .
N1 P1 C1 106.83(17) . .
N1 P1 C2 110.08(13) . .
C1 P1 C2 110.14(18) . .
N1 P1 C8 110.27(15) . .
C1 P1 C8 114.41(16) . .
C2 P1 C8 105.13(14) . .
C3 C2 C7 118.3(3) . .
C3 C2 P1 124.8(2) . .
C7 C2 P1 116.9(2) . .
C2 C3 C4 121.5(3) . .
C5 C4 C3 119.2(3) . .
C6 C5 C4 120.1(3) . .
C7 C6 C5 120.2(3) . .
C6 C7 C2 120.7(3) . .
C13 C8 C9 119.7(3) . .
C13 C8 P1 120.9(3) . .
C9 C8 P1 119.1(3) . .
C8 C9 C10 120.3(4) . .
C11 C10 C9 119.7(4) . .
C10 C11 C12 120.3(3) . .
C11 C12 C13 119.6(4) . .
C8 C13 C12 120.3(4) . .
P1 N1 Si1 130.95(15) . .
P1 N1 Er1 92.69(9) . .
Si1 N1 Er1 132.65(13) . .
N1 Si1 C14 111.99(14) . .
N1 Si1 C16 106.91(14) . .
C14 Si1 C16 108.38(19) . .
N1 Si1 C15 113.64(14) . .
C14 Si1 C15 107.16(17) . .
C16 Si1 C15 108.63(19) . .
C18 C17 Er1 101.0(3) . .
C19 C18 C19 114.9(5) 4_575 .
C19 C18 C17 122.4(3) 4_575 .
C19 C18 C17 122.4(3) . .
C20 C19 C18 122.2(4) . .
C19 C20 C21 120.9(4) . .
C20 C21 C20 118.7(6) 4_575 .
C22 O1 C25 109.9(4) . .
C22 O1 Er1 130.8(3) . .
C25 O1 Er1 119.3(3) . .
O1 C22 C23 104.6(12) . .
C22 C23 C24 105.0(14) . .
C23 C24 C25 99.8(16) . .
O1 C25 C24 107.7(9) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Er1 N1 2.330(2) .
Er1 N1 2.330(2) 4_575
Er1 C1 2.339(4) .
Er1 O1 2.341(3) .
Er1 C17 2.379(5) .
C1 P1 1.6575(14) .
C1 P1 1.6575(14) 4_575
P1 N1 1.623(3) .
P1 C2 1.823(3) .
P1 C8 1.829(3) .
C2 C3 1.371(4) .
C2 C7 1.406(5) .
C3 C4 1.399(5) .
C4 C5 1.383(5) .
C5 C6 1.382(5) .
C6 C7 1.379(5) .
C8 C13 1.365(5) .
C8 C9 1.385(5) .
C9 C10 1.396(5) .
C10 C11 1.374(6) .
C11 C12 1.375(7) .
C12 C13 1.408(5) .
N1 Si1 1.721(2) .
Si1 C14 1.867(4) .
Si1 C16 1.869(4) .
Si1 C15 1.882(3) .
C17 C18 1.443(7) .
C18 C19 1.411(5) 4_575
C18 C19 1.411(5) .
C19 C20 1.370(6) .
C20 C21 1.373(5) .
C21 C20 1.373(5) 4_575
O1 C22 1.436(3) .
O1 C25 1.437(3) .
C22 C23 1.505(5) .
C23 C24 1.524(5) .
C24 C25 1.525(5) .
C23A C24A 1.524(5) .
