Rare-earth metal ethylene and ethyne complexes.
Jiang, Wen; Rajeshkumar, Thayalan; Guo, Mengyue; Lin, Yuejian; Maron, Laurent; Zhang, Lixin; Chemical science 15 (2024) 3495–3501; doi:10.1039/d3sc06599e

data_1570851
_publ_section_title
;
 Rare-earth metal ethylene and ethyne complexes.
;
_journal_issue                   10
_journal_name_full               'Chemical science'
_journal_page_first              3495
_journal_page_last               3501
_journal_paper_doi               10.1039/d3sc06599e
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         '2(C43 H58 Lu N3), C7 H8'
_chemical_formula_sum            'C93 H124 Lu2 N6'
_chemical_formula_weight         1675.91
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-04-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-04-28 deposited with the CCDC.	2024-01-30 downloaded from the CCDC.
;
_cell_angle_alpha                87.0960(10)
_cell_angle_beta                 78.3860(10)
_cell_angle_gamma                85.535(2)
_cell_formula_units_Z            2
_cell_length_a                   10.8568(4)
_cell_length_b                   19.2449(8)
_cell_length_c                   21.6617(7)
_cell_measurement_reflns_used    9764
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.06
_cell_measurement_theta_min      2.26
_cell_volume                     4417.0(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1023
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            307106
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.500
_diffrn_reflns_theta_min         2.228
_exptl_absorpt_coefficient_mu    2.267
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6262
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_description       block
_exptl_crystal_F_000             1732
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
TITL mo_210823b_a.res in P-1
CELL   10.8568   19.2449   21.6617     87.10     78.39     85.54
SPGR P-1
C101 0.592 0.501 0.460 !       3.76 eA-3
C102 0.173 0.594 0.405 !       3.04 eA-3
C103 0.249 0.531 0.396 !       2.60 eA-3
C104 0.471 0.499 0.482 !       2.29 eA-3
C105 0.324 0.500 0.497 !       2.28 eA-3
C106 0.386 0.513 0.425 !       2.28 eA-3
C107 0.502 0.501 0.421 !       2.15 eA-3
C108 0.107 0.604 0.459 !       1.97 eA-3
C109 0.328 0.531 0.332 !       1.95 eA-3
C110 0.044 0.548 0.493 !       1.86 eA-3
C111 0.219 0.469 0.403 !       1.82 eA-3
C112 0.110 0.563 0.457 !       1.79 eA-3
C113 0.285 0.580 0.350 !       1.68 eA-3
C114 0.080 0.489 0.483 !       1.42 eA-3
C115 0.172 0.480 0.435 !       1.26 eA-3
Q116 0.505 0.858 0.104 !       1.24 eA-3
C117 0.143 0.440 0.457 !       1.18 eA-3
Q118 0.437 0.816 0.082 !       1.17 eA-3
Q119 0.636 0.999 0.397 !       1.10 eA-3
C120 0.159 0.595 0.485 !       1.01 eA-3
Q121 0.339 0.764 0.182 !       1.01 eA-3
C122 0.813 0.409 0.480 !       0.98 eA-3
Q123 0.485 0.864 0.166 !       0.96 eA-3
Q124 0.763 0.958 0.278 !       0.90 eA-3
Q125 0.143 0.377 0.077 !       0.80 eA-3
C126 0.779 0.469 0.493 !       0.77 eA-3
C127 0.880 0.441 0.480 !       0.77 eA-3
C128 0.793 0.505 0.481 !       0.76 eA-3
C129 0.276 0.624 0.371 !       0.72 eA-3
Q130 0.794 0.449 0.381 !       0.71 eA-3
C131 0.985 0.361 0.499 !       0.70 eA-3
Q132 0.750 0.894 0.427 !       0.70 eA-3
Q133 0.469 0.031 0.052 !       0.69 eA-3
Q134 0.535 0.968 0.468 !       0.68 eA-3
Q135 0.392 0.578 0.337 !       0.68 eA-3
Q136 0.483 0.064 0.431 !       0.67 eA-3
Q137 0.377 0.809 0.202 !       0.64 eA-3
Q138 0.592 1.000 0.461 !       0.63 eA-3
Q139 0.606 0.031 0.029 !       0.63 eA-3
Q140 0.575 0.012 0.043 !       0.63 eA-3
Q141 0.654 0.375 0.040 !       0.63 eA-3
Q142 0.933 0.457 0.107 !       0.63 eA-3
Q143 0.436 0.921 0.008 !       0.63 eA-3
C144 0.627 0.452 0.508 !       0.62 eA-3
Q145 0.965 0.409 0.229 !       0.62 eA-3
Q146 0.580 0.907 0.194 !       0.61 eA-3
C147 0.152 0.659 0.427 !       0.61 eA-3
Q148 0.981 0.686 0.105 !       0.61 eA-3
Q149 0.058 0.499 0.063 !       0.60 eA-3
Q150 0.475 0.035 0.478 !       0.60 eA-3
Q151 0.845 0.580 0.032 !       0.59 eA-3
Q152 0.373 0.814 0.404 !       0.59 eA-3
C153 0.707 0.423 0.502 !       0.57 eA-3
Q154 0.610 0.159 0.412 !       0.56 eA-3
C155 0.645 0.502 0.411 !       0.56 eA-3
C156 0.283 0.566 0.307 !       0.56 eA-3
C157 0.203 0.639 0.377 !       0.56 eA-3
Q158 0.331 0.999 0.015 !       0.55 eA-3
Q159 0.970 0.439 0.452 !       0.55 eA-3
C160 0.034 0.609 0.441 !       0.55 eA-3
Q161 0.032 0.475 0.030 !       0.55 eA-3
Q162 0.997 0.689 0.479 !       0.55 eA-3
Q163 0.767 0.390 0.174 !       0.55 eA-3
Q164 0.313 0.622 0.422 !       0.54 eA-3
Q165 0.580 0.889 0.415 !       0.54 eA-3
Q166 0.857 0.373 0.149 !       0.54 eA-3
Q167 0.454 0.473 0.420 !       0.54 eA-3
Q168 0.409 0.984 0.017 !       0.53 eA-3
Q169 0.389 0.092 0.417 !       0.53 eA-3
Q170 0.968 0.423 0.079 !       0.53 eA-3
Q171 0.252 0.998 0.261 !       0.52 eA-3
Q172 0.810 1.002 0.169 !       0.52 eA-3
Q173 0.440 0.108 0.448 !       0.52 eA-3
Q174 0.861 0.546 0.046 !       0.52 eA-3
C175 0.717 0.533 0.447 !       0.52 eA-3
C176 0.248 0.611 0.317 !       0.51 eA-3
Q177 0.561 0.031 0.268 !       0.51 eA-3
Q178 0.596 0.890 0.344 !       0.51 eA-3
Q179 0.623 0.082 0.099 !       0.51 eA-3
Q180 0.723 0.139 0.132 !       0.51 eA-3
Q181 0.500 1.000 0.000 !       0.51 eA-3
Q182 0.451 0.608 0.339 !       0.51 eA-3
Q183 0.828 0.593 0.079 !       0.51 eA-3
C184 0.123 0.390 0.457 !       0.50 eA-3
Q185 0.215 0.816 0.353 !       0.50 eA-3
;
_refine_diff_density_max         1.114
_refine_diff_density_min         -0.907
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     968
_refine_ls_number_reflns         18302
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0311
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0259P)^2^+8.3422P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0670
_refine_ls_wR_factor_ref         0.0726
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14759
_reflns_number_total             18302
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc06599e2.cif
_cod_data_source_block           platon_sq
_cod_depositor_comments
'Adding full bibliography for 1570851--1570856.cif.'
_cod_database_code               1570851
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.895
_shelx_estimated_absorpt_t_min   0.612
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All H(H) groups, All C(H,H,H) groups
2. Restrained distances
 H3A-H3B
 1.6 with sigma of 0.03
 C3-H3A = C3-H3B = C4-H4A = C4-H4B = C4-H4C
 0.99 with sigma of 0.02
 C46-H46A = C46-H46B = C47-H47A = C47-H47B = C47-H47C
 1.03 with sigma of 0.05
3.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C24(H24), C27(H27), C55(H55), C58(H58), C67(H67), C70(H70)
3.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C30(H30A,H30B), C37(H37A,H37B), C44(H44A,H44B), C73(H73A,H73B),
 C80(H80A,H80B)
3.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22), C32(H32), C33(H33),
 C34(H34), C35(H35), C36(H36), C39(H39), C40(H40), C41(H41), C42(H42), C43(H43),
  C51(H51), C52(H52), C53(H53), C63(H63), C64(H64), C65(H65), C75(H75),
 C76(H76), C77(H77), C78(H78), C79(H79), C82(H82), C83(H83), C84(H84), C85(H85),
  C86(H86), C89(H89), C90(H90), C91(H91), C92(H92), C93(H93)
3.d Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C16(H16A,H16B,
 H16C), C17(H17A,H17B,H17C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C28(H28A,
 H28B,H28C), C29(H29A,H29B,H29C), C45(H45A,H45B,H45C), C56(H56A,H56B,H56C),
 C57(H57A,H57B,H57C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C68(H68A,H68B,
 H68C), C69(H69A,H69B,H69C), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C), C87(H87A,
 H87B,H87C)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'