#------------------------------------------------------------------------------
#$Date: 2018-09-12 16:47:12 +0200 (Wed 12 de Sep de 2018) $
#$Revision: 210898 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/67/7116724.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_7116724
loop_
_publ_author_name
'Rong, Weifeng'
'He, Dongliang'
'Wang, Meiyan'
'Mou, Zehuai'
'Cheng, Jianhua'
'Yao, Changguang'
'Li, Shihui'
'Trifonov, Alexander A.'
'Lyubov, Dmitrii M.'
'Cui, Dongmei'
_publ_section_title
;
 Neutral binuclear rare-earth metal complexes with four μ2-bridging hydrides
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   24
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              5063
_journal_page_last               5065
_journal_paper_doi               10.1039/c4cc07262f
_journal_volume                  51
_journal_year                    2015
_chemical_formula_sum            'C48 H56 Lu N3 P2'
_chemical_formula_weight         911.87
_space_group_IT_number           23
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'I 2 2'
_symmetry_space_group_name_H-M   'I 2 2 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2014-08-19 deposited with the CCDC.
2015-02-11 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.164(2)
_cell_length_b                   18.573(3)
_cell_length_c                   19.615(3)
_cell_measurement_reflns_used    1291
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15.54
_cell_measurement_theta_min      2.19
_cell_volume                     4795.8(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1187
_diffrn_reflns_av_sigmaI/netI    0.1357
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            13567
_diffrn_reflns_theta_full        25.11
_diffrn_reflns_theta_max         25.11
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    2.157
_exptl_absorpt_correction_T_max  0.7973
_exptl_absorpt_correction_T_min  0.6722
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1864
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_platon_squeeze_details
;
;
_refine_diff_density_max         2.929
_refine_diff_density_min         -2.176
_refine_diff_density_rms         0.175
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.40(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         4256
_refine_ls_number_restraints     62
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1568
_refine_ls_R_factor_gt           0.1179
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1202P)²+92.5974P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2619
_refine_ls_wR_factor_ref         0.2889
_reflns_number_gt                2862
_reflns_number_total             4256
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc07262f2-1c.cif
_cod_data_source_block           x226
_cod_original_sg_symbol_H-M      I222
_cod_database_code               7116724
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
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
Lu1 Lu 1.0000 0.58356(7) 1.0000 0.1056(9) Uani 1 2 d S
H1 H 0.9251 0.5018 1.0503 0.06(4) Uiso 1 1 d R
P1 P 0.9092(3) 0.7201(2) 0.9482(2) 0.0360(9) Uani 1 1 d .
N1 N 1.0000 0.7185(8) 1.0000 0.038(2) Uani 1 2 d SU
N2 N 0.9097(10) 0.6398(7) 0.9166(7) 0.038(2) Uani 1 1 d U
C1 C 0.9234(12) 0.7905(8) 0.8868(7) 0.033(3) Uani 1 1 d U
C2 C 1.003(3) 0.8403(11) 0.8903(9) 0.082(7) Uani 1 1 d .
H2 H 1.0489 0.8354 0.9263 0.099 Uiso 1 1 calc R
C3 C 1.0209(13) 0.8957(8) 0.8453(8) 0.045(4) Uani 1 1 d U
H3 H 1.0766 0.9262 0.8486 0.054 Uiso 1 1 calc R
C4 C 0.9451(15) 0.9022(11) 0.7928(10) 0.064(6) Uani 1 1 d .
H4 H 0.9494 0.9397 0.7615 0.077 Uiso 1 1 calc R
C5 C 0.8683(19) 0.8550(13) 0.7882(11) 0.081(7) Uani 1 1 d .
H5 H 0.8231 0.8604 0.7522 0.098 Uiso 1 1 calc R
C6 C 0.8517(16) 0.7996(11) 0.8327(10) 0.060(6) Uani 1 1 d .
H6 H 0.7961 0.7691 0.8280 0.072 Uiso 1 1 calc R
C7 C 0.7977(15) 0.7418(11) 0.9959(12) 0.067(6) Uani 1 1 d .
C8 C 0.739(2) 0.7992(11) 0.990(2) 0.122(13) Uani 1 1 d .
H8 H 0.7588 0.8349 0.9593 0.147 Uiso 1 1 calc R
C9 C 0.646(3) 0.809(2) 1.029(2) 0.139(13) Uani 1 1 d U
H9 H 0.6036 0.8480 1.0193 0.167 Uiso 1 1 calc R
C10 C 0.622(4) 0.764(2) 1.076(2) 0.175(19) Uani 1 1 d U
H10 H 0.5673 0.7736 1.1042 0.210 Uiso 1 1 calc R
C11 C 0.672(3) 0.705(2) 1.0854(17) 0.114(10) Uani 1 1 d U
H11 H 0.6489 0.6717 1.1169 0.137 Uiso 1 1 calc R
C12 C 0.7662(17) 0.6917(16) 1.0462(14) 0.093(8) Uani 1 1 d .
H12 H 0.8044 0.6505 1.0546 0.111 Uiso 1 1 calc R
C13 C 0.8703(13) 0.6243(9) 0.8509(7) 0.040(4) Uani 1 1 d .
C14 C 0.7689(13) 0.6029(9) 0.8420(8) 0.046(4) Uani 1 1 d .
C15 C 0.7325(15) 0.5926(13) 0.7763(8) 0.067(6) Uani 1 1 d .
H15 H 0.6659 0.5769 0.7710 0.081 Uiso 1 1 calc R
C16 C 0.7876(14) 0.6040(10) 0.7209(10) 0.053(5) Uani 1 1 d U
H16 H 0.7586 0.6007 0.6778 0.064 Uiso 1 1 calc R
C17 C 0.8892(17) 0.6209(12) 0.7284(8) 0.069(6) Uani 1 1 d .
H17 H 0.9307 0.6249 0.6902 0.083 Uiso 1 1 calc R
C18 C 0.9276(12) 0.6314(9) 0.7903(8) 0.039(4) Uani 1 1 d U
C19 C 0.6952(15) 0.5857(13) 0.9024(10) 0.065(5) Uani 1 1 d U
H19 H 0.7328 0.5933 0.9449 0.077 Uiso 1 1 calc R
C20 C 0.661(2) 0.5108(18) 0.9016(12) 0.092(8) Uani 1 1 d .
H20A H 0.7190 0.4795 0.9053 0.138 Uiso 1 1 calc R
H20B H 0.6261 0.5012 0.8597 0.138 Uiso 1 1 calc R
H20C H 0.6162 0.5026 0.9394 0.138 Uiso 1 1 calc R
C21 C 0.6058(17) 0.6389(17) 0.9017(14) 0.097(8) Uani 1 1 d U
H21A H 0.5697 0.6359 0.9442 0.146 Uiso 1 1 calc R
H21B H 0.5607 0.6272 0.8649 0.146 Uiso 1 1 calc R
H21C H 0.6311 0.6870 0.8957 0.146 Uiso 1 1 calc R
C22 C 1.0392(11) 0.6491(9) 0.8022(10) 0.044(4) Uani 1 1 d .
H22 H 1.0465 0.6683 0.8485 0.053 Uiso 1 1 calc R
C23 C 1.0797(13) 0.7075(11) 0.7502(11) 0.066(6) Uani 1 1 d U
H23A H 1.0427 0.7516 0.7563 0.098 Uiso 1 1 calc R
H23B H 1.0703 0.6904 0.7044 0.098 Uiso 1 1 calc R
H23C H 1.1506 0.7159 0.7583 0.098 Uiso 1 1 calc R
C24 C 1.1067(15) 0.5791(13) 0.7960(15) 0.090(8) Uani 1 1 d .
H24A H 1.1243 0.5713 0.7491 0.135 Uiso 1 1 calc R
H24B H 1.0693 0.5384 0.8128 0.135 Uiso 1 1 calc R
H24C H 1.1675 0.5850 0.8225 0.135 Uiso 1 1 calc R
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Lu Lu -0.4720 5.8584 '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
N2 Lu1 N2 125.3(7) 3_757 .
N2 Lu1 N1 62.7(3) 3_757 .
N2 Lu1 N1 62.7(3) . .
N2 Lu1 P1 32.4(3) 3_757 3_757
N2 Lu1 P1 93.6(3) . 3_757
N1 Lu1 P1 31.73(7) . 3_757
N2 Lu1 Lu1 117.3(3) 3_757 2_765
N2 Lu1 Lu1 117.3(3) . 2_765
N1 Lu1 Lu1 180.0 . 2_765
P1 Lu1 Lu1 148.27(7) 3_757 2_765
N2 Lu1 H1 104.1 3_757 .
N2 Lu1 H1 115.6 . .
N1 Lu1 H1 137.4 . .
P1 Lu1 H1 130.9 3_757 .
Lu1 Lu1 H1 42.6 2_765 .
N1 P1 N2 103.2(7) . .
N1 P1 C1 111.8(7) . .
N2 P1 C1 114.6(7) . .
N1 P1 C7 106.9(8) . .
N2 P1 C7 114.4(8) . .
C1 P1 C7 105.9(9) . .
P1 N1 P1 177.8(11) 3_757 .
P1 N1 Lu1 91.1(6) 3_757 .
P1 N1 Lu1 91.1(6) . .
C13 N2 P1 122.4(11) . .
C13 N2 Lu1 138.6(10) . .
P1 N2 Lu1 98.6(6) . .
C2 C1 C6 117.0(16) . .
C2 C1 P1 121.8(12) . .
C6 C1 P1 121.1(12) . .
C3 C2 C1 126(2) . .
C3 C2 H2 117.0 . .
C1 C2 H2 117.0 . .
C2 C3 C4 114.1(19) . .
C2 C3 H3 123.0 . .
C4 C3 H3 123.0 . .
C5 C4 C3 120.9(18) . .
C5 C4 H4 119.5 . .
C3 C4 H4 119.5 . .
C4 C5 C6 125(2) . .
C4 C5 H5 117.6 . .
C6 C5 H5 117.6 . .
C5 C6 C1 117.2(17) . .
C5 C6 H6 121.4 . .
C1 C6 H6 121.4 . .
C8 C7 C12 115(2) . .
C8 C7 P1 128(2) . .
C12 C7 P1 117.2(19) . .
C7 C8 C9 123(3) . .
C7 C8 H8 118.5 . .
C9 C8 H8 118.5 . .
C10 C9 C8 120(4) . .
C10 C9 H9 120.2 . .
C8 C9 H9 120.2 . .
C9 C10 C11 122(4) . .
C9 C10 H10 118.9 . .
C11 C10 H10 118.8 . .
C12 C11 C10 120(4) . .
C12 C11 H11 120.0 . .
C10 C11 H11 120.0 . .
C11 C12 C7 119(3) . .
C11 C12 H12 120.3 . .
C7 C12 H12 120.2 . .
C14 C13 C18 115.4(13) . .
C14 C13 N2 121.3(15) . .
C18 C13 N2 123.3(15) . .
C15 C14 C13 118.9(16) . .
C15 C14 C19 117.4(16) . .
C13 C14 C19 123.6(14) . .
C16 C15 C14 123.4(19) . .
C16 C15 H15 118.3 . .
C14 C15 H15 118.3 . .
C15 C16 C17 118.6(17) . .
C15 C16 H16 120.7 . .
C17 C16 H16 120.7 . .
C18 C17 C16 119.9(18) . .
C18 C17 H17 120.0 . .
C16 C17 H17 120.0 . .
C17 C18 C13 123.4(16) . .
C17 C18 C22 122.5(17) . .
C13 C18 C22 114.0(14) . .
C20 C19 C21 112(2) . .
C20 C19 C14 112.2(18) . .
C21 C19 C14 109.7(18) . .
C20 C19 H19 107.5 . .
C21 C19 H19 107.5 . .
C14 C19 H19 107.5 . .
C19 C20 H20A 109.5 . .
C19 C20 H20B 109.5 . .
H20A C20 H20B 109.5 . .
C19 C20 H20C 109.5 . .
H20A C20 H20C 109.5 . .
H20B C20 H20C 109.5 . .
C19 C21 H21A 109.5 . .
C19 C21 H21B 109.5 . .
H21A C21 H21B 109.5 . .
C19 C21 H21C 109.5 . .
H21A C21 H21C 109.5 . .
H21B C21 H21C 109.5 . .
C18 C22 C23 112.0(14) . .
C18 C22 C24 110.7(16) . .
C23 C22 C24 109.0(15) . .
C18 C22 H22 108.3 . .
C23 C22 H22 108.3 . .
C24 C22 H22 108.3 . .
C22 C23 H23A 109.5 . .
C22 C23 H23B 109.5 . .
H23A C23 H23B 109.5 . .
C22 C23 H23C 109.5 . .
H23A C23 H23C 109.5 . .
H23B C23 H23C 109.5 . .
C22 C24 H24A 109.5 . .
C22 C24 H24B 109.5 . .
H24A C24 H24B 109.5 . .
C22 C24 H24C 109.5 . .
H24A C24 H24C 109.5 . .
H24B C24 H24C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Lu1 N2 2.276(12) 3_757
Lu1 N2 2.276(12) .
Lu1 N1 2.507(15) .
Lu1 P1 2.982(4) 3_757
Lu1 Lu1 3.104(3) 2_765
Lu1 H1 2.0622 .
P1 N1 1.569(4) .
P1 N2 1.615(13) .
P1 C1 1.787(17) .
P1 C7 1.79(2) .
N1 P1 1.569(4) 3_757
N2 C13 1.419(18) .
C1 C2 1.40(3) .
C1 C6 1.43(2) .
C2 C3 1.37(2) .
C2 H2 0.9300 .
C3 C4 1.44(2) .
C3 H3 0.9300 .
C4 C5 1.34(3) .
C4 H4 0.9300 .
C5 C6 1.37(3) .
C5 H5 0.9300 .
C6 H6 0.9300 .
C7 C8 1.32(3) .
C7 C12 1.42(4) .
C8 C9 1.46(4) .
C8 H8 0.9300 .
C9 C10 1.30(5) .
C9 H9 0.9300 .
C10 C11 1.28(5) .
C10 H10 0.9300 .
C11 C12 1.48(4) .
C11 H11 0.9300 .
C12 H12 0.9300 .
C13 C14 1.40(2) .
C13 C18 1.41(2) .
C14 C15 1.39(2) .
C14 C19 1.56(2) .
C15 C16 1.33(3) .
C15 H15 0.9300 .
C16 C17 1.38(3) .
C16 H16 0.9300 .
C17 C18 1.33(2) .
C17 H17 0.9300 .
C18 C22 1.52(2) .
C19 C20 1.46(4) .
C19 C21 1.54(3) .
C19 H19 0.9800 .
C20 H20A 0.9600 .
C20 H20B 0.9600 .
C20 H20C 0.9600 .
C21 H21A 0.9600 .
C21 H21B 0.9600 .
C21 H21C 0.9600 .
C22 C23 1.58(3) .
C22 C24 1.58(3) .
C22 H22 0.9800 .
C23 H23A 0.9600 .
C23 H23B 0.9600 .
C23 H23C 0.9600 .
C24 H24A 0.9600 .
C24 H24B 0.9600 .
C24 H24C 0.9600 .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.014 0.000 0.000 361 111 ' '
2 -0.007 0.500 0.500 361 111 ' '
