Rigid NON-donor pincer ligand complexes of lutetium and lanthanum: synthesis and hydroamination catalysis
Motolko, Kelly S. A.; Emslie, David J. H.; Britten, James F.; RSC Adv. 7 (2017) 27938–; doi:10.1039/C7RA04432A

data_7228336
_publ_section_title
;
 Rigid NON-donor pincer ligand complexes of lutetium and lanthanum:
 synthesis and hydroamination catalysis
;
_journal_issue                   45
_journal_name_full               'RSC Adv.'
_journal_page_first              27938
_journal_paper_doi               10.1039/C7RA04432A
_journal_volume                  7
_journal_year                    2017
_chemical_formula_moiety         '4(C61 H93 Lu N2 O2 Si), 2(C6 H6)'
_chemical_formula_sum            'C256 H384 Lu4 N8 O8 Si4'
_chemical_formula_weight         4513.93
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-02-17
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2017-04-19 deposited with the CCDC.
2017-05-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.6878(11)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   22.6630(5)
_cell_length_b                   14.5298(3)
_cell_length_c                   20.3925(4)
_cell_measurement_reflns_used    9924
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.622
_cell_measurement_theta_min      2.273
_cell_volume                     6149.3(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_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  0.0468
_diffrn_reflns_av_unetI/netI     0.0235
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            207822
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         2.593
_exptl_absorpt_coefficient_mu    1.666
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6309
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
'SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0636 before and 0.0464 after correction.
The Ratio of minimum to maximum transmission is 0.8453.
The \l/2 correction factor is 0.00150.'
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_description       rod
_exptl_crystal_F_000             2380
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.198
_refine_diff_density_min         -0.716
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     660
_refine_ls_number_reflns         18762
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0286
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0328P)^2^+5.0472P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0652
_refine_ls_wR_factor_ref         0.0704
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15662
_reflns_number_total             18762
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra04432a2.cif
_cod_data_source_block           xn2luch2sime3_0m
_cod_database_code               7228336
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.892
_shelx_estimated_absorpt_t_min   0.555
_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. Shared sites
{C16, C16A}
3. Uiso/Uaniso restraints and constraints
Uanis(C16) = Uanis(C16A)
4. Same fragment restrains
{C16A, C17A, C18A, C19A} sigma for 1-2: 0.002, 1-3: 0.004
as
{C16, C17, C18, C19}
5. Others
 Sof(C16A)=Sof(C17A)=Sof(H17D)=Sof(H17E)=Sof(H17F)=Sof(C18A)=Sof(H18D)=
 Sof(H18E)=Sof(H18F)=Sof(C19A)=Sof(H19D)=Sof(H19E)=Sof(H19F)=1-FVAR(1)
 Sof(C16)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C18)=Sof(H18A)=Sof(H18B)=
 Sof(H18C)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C30(H30), C33(H33), C36(H36), C45(H45), C48(H48), C51(H51)
6.b Secondary CH2 refined with riding coordinates:
 C54(H54A,H54B), C58(H58A,H58B), C59(H59A,H59B), C60(H60A,H60B), C61(H61A,H61B)
6.c Me refined with riding coordinates:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C19(H19A,H19B,H19C), C17A(H17D,H17E,H17F), C18A(H18D,H18E,H18F),
 C19A(H19D,H19E,H19F), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C35(H35A,
 H35B,H35C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C47(H47A,H47B,H47C),
 C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C52(H52A,H52B,H52C), C53(H53A,H53B,
 H53C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C)
6.d Me refined as rotating group:
 C46(H46A,H46B,H46C)
6.e Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C6(H6), C8(H8), C26(H26), C28(H28), C41(H41), C43(H43),
 C62(H62), C63(H63), C64(H64)
;
_shelx_res_checksum              21373
_olex2_submission_original_sample_id C61H93N2O2LuSi
_olex2_submission_special_instructions 'No special instructions were received'