A (C<sub>5</sub>Me<sub>5</sub>)/enolamido lutetium dinitrogen complex promoted by deprotonation on the amidinate ligand.
Chen, Xiao; Xu, Hanhua; Xi, Zhenfeng; Wei, Junnian; Chemical communications (Cambridge, England) 60 (2024) 12750–12753; doi:10.1039/d4cc04338c

data_7133936
_publ_section_title
;
 A (C<sub>5</sub>Me<sub>5</sub>)/enolamido lutetium dinitrogen complex
 promoted by deprotonation on the amidinate ligand.
;
_journal_issue                   87
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              12750
_journal_page_last               12753
_journal_paper_doi               10.1039/d4cc04338c
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety
'C56 H92 K2 Lu2 N6, 2(C18 H36 K N2 O6), 2(C4 H8 O)'
_chemical_formula_sum            'C100 H180 K4 Lu2 N10 O14'
_chemical_formula_weight         2252.87
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive
_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     dual
_audit_creation_date             2024-05-06
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-08-24 deposited with the CCDC.	2024-10-07 downloaded from the CCDC.
;
_cell_angle_alpha                113.745(2)
_cell_angle_beta                 95.077(2)
_cell_angle_gamma                102.135(2)
_cell_formula_units_Z            1
_cell_length_a                   12.4692(3)
_cell_length_b                   16.0421(4)
_cell_length_c                   16.7103(4)
_cell_measurement_reflns_used    29966
_cell_measurement_temperature    179.99(10)
_cell_measurement_theta_max      30.2690
_cell_measurement_theta_min      2.2510
_cell_volume                     2934.75(14)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      179.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.874
_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    -14.00  92.00   0.50    7.64    --    4.30  57.00  30.00  212
  2  \w    -27.00  74.00   0.50    7.64    --    4.30  77.00-120.00  202
  3  \w    -22.00  81.00   0.50    7.64    --    4.30  57.00-180.00  206
  4  \w    -12.00  22.00   0.50    7.64    --    4.30  77.00 -60.00   68
  5  \w    -84.00 -59.00   0.50    7.64    --    4.30 -57.00 -60.00   50
  6  \w     10.00  80.00   0.50    7.64    --    4.30  19.00  30.00  140
  7  \w    -85.00  39.00   0.50    7.64    --    4.30 -19.00  60.00  248
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_unetI/netI     0.0281
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.874
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_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            61077
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.874
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.211
_diffrn_reflns_theta_min         2.368
_exptl_absorpt_coefficient_mu    1.871
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68040
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_description       block
_exptl_crystal_F_000             1180
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.137
_refine_diff_density_min         -0.754
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     639
_refine_ls_number_reflns         15258
_refine_ls_number_restraints     305
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0282
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0413P)^2^+0.8932P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0687
_refine_ls_wR_factor_ref         0.0727
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13080
_reflns_number_total             15258
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc04338c6.cif
_cod_data_source_block           a
_cod_original_cell_volume        2934.74(13)
_cod_database_code               7133936
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.729
_shelx_estimated_absorpt_t_min   0.673
_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 C(H,H,H) groups
2. Restrained distances
 C50-O7 = O7-C47
 1.43 with sigma of 0.02
 C50A-C49A = C47A-C48A
 1.54 with sigma of 0.02
 C50-C49 = C47-C48
 1.54 with sigma of 0.02
 C50A-O7A = O7A-C47A
 1.43 with sigma of 0.02
 O7A-C47A = O7A-C50A
 1.43 with sigma of 0.01
 O7-C47 = O7-C50
 1.43 with sigma of 0.01
 C49A-C48A
 1.54 with sigma of 0.01
 C50-C47 = C50A-C47A
 2.336 with sigma of 0.04
 C50-C48 = C47-C49
 2.515 with sigma of 0.04
 C47A-C49A = C50A-C48A
 2.515 with sigma of 0.04
 O7-C49 = O7-C48
 2.426 with sigma of 0.04
 O7A-C49A = O7A-C48A
 2.426 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
O7 \\sim C47 \\sim C48 \\sim C49 \\sim C50 \\sim O7A \\sim C47A \\sim C48A
\\sim C49A \\sim C50A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
Uanis(O7A) \\sim Ueq, Uanis(C47A) \\sim Ueq, Uanis(C50A) \\sim Ueq, Uanis(C48A)
\\sim Ueq, Uanis(C49A) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(C47) \\sim Ueq,
Uanis(C50) \\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C49) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 O7, C47, C48, C49, C50, O7A, C47A, C48A, C49A, C50A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
5. Others
 Sof(O7A)=Sof(C47A)=Sof(H47C)=Sof(H47D)=Sof(C48A)=Sof(H48C)=Sof(H48D)=
 Sof(C49A)=Sof(H49C)=Sof(H49D)=Sof(C50A)=Sof(H50C)=Sof(H50D)=1-FVAR(1)
 Sof(O7)=Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(C49)=
 Sof(H49A)=Sof(H49B)=Sof(C50)=Sof(H50A)=Sof(H50B)=FVAR(1)
 Fixed X: C47A(0.92702)
 Fixed Y: Lu1(0.91056)
 Fixed Z: Lu1(0.521371)
6.a Riding coordinates:
 C1(H1A,H1B,H1C), C7(H7A,H7B,H7C), C11(H11A,H11B,H11C), C14(H14A,H14B,H14C)
6.b Ternary CH refined with riding coordinates:
 C12(H12), C15(H15)
6.c Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,
 H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B),
 C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B),
  C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,
 H47B), C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B), C47A(H47C,H47D),
 C48A(H48C,H48D), C49A(H49C,H49D), C50A(H50C,H50D)
6.d X=CH2 refined with riding coordinates:
 C17(H17A,H17B)
6.e Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C13(H13A,H13B,H13C),
 C16(H16A,H16B,H16C), C19(H19A,H19B,H19C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C)
;
_shelx_res_checksum              83984
_shelx_hkl_checksum              57393
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;