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_7228335
_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         'C61 H96 La N2 O Si2, C16 H32 Li O4, C4 H8 O'
_chemical_formula_sum            'C81 H136 La Li N2 O6 Si2'
_chemical_formula_weight         1435.94
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-01-20
_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                 98.980(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.931(2)
_cell_length_b                   23.782(3)
_cell_length_c                   21.090(3)
_cell_measurement_reflns_used    9304
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      26.17
_cell_measurement_theta_min      2.30
_cell_volume                     8387.9(19)
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.991
_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  0.0529
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            120442
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.460
_diffrn_reflns_theta_min         1.299
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.585
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6493
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
'SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0660 before and 0.0539 after correction.
The Ratio of minimum to maximum transmission is 0.8711.
The \l/2 correction factor is 0.00150.'
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.137
_exptl_crystal_description       block
_exptl_crystal_F_000             3088
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.550
_refine_diff_density_min         -1.638
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     843
_refine_ls_number_reflns         17160
_refine_ls_number_restraints     929
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.1057
_refine_ls_R_factor_gt           0.0840
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1160P)^2^+57.0794P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2367
_refine_ls_wR_factor_ref         0.2570
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13364
_reflns_number_total             17160
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra04432a2.cif
_cod_data_source_block           xn2lab
_cod_original_cell_volume        8388(2)
_cod_database_code               7228335
_shelx_shelxl_version_number     2014/7
_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
{O5, O5A}
3. Uiso/Uaniso restraints and constraints
Uanis(C74) = Uanis(C74A)
Uanis(C75) = Uanis(C75A)
Uanis(C76) = Uanis(C76A)
Uanis(C77) = Uanis(C77A)
Uanis(O5) = Uanis(O5A)
Uanis(La1) = Uanis(La1A) = Uanis(La1B)
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{O3, C66, C67, C68, C69} sigma for 1-2: 0.001, 1-3: 0.002
{O4, C70, C71, C72, C73} sigma for 1-2: 0.001, 1-3: 0.002
{O5, C74, C75, C76, C77} sigma for 1-2: 0.001, 1-3: 0.002
{O5A, C74A, C75A, C76A, C77A} sigma for 1-2: 0.001, 1-3: 0.002
as
{O2, C62, C63, C64, C65}
6. Others
 1*[Sof(La1)]+1*[Sof(La1A)]+1*[Sof(La1B)]=1 with esd of 0.001
 Sof(O5A)=Sof(C74A)=Sof(H74C)=Sof(H74D)=Sof(C75A)=Sof(H75C)=Sof(H75D)=
 Sof(C76A)=Sof(H76C)=Sof(H76D)=Sof(C77A)=Sof(H77C)=Sof(H77D)=1-FVAR(1)
 Sof(O5)=Sof(C74)=Sof(H74A)=Sof(H74B)=Sof(C75)=Sof(H75A)=Sof(H75B)=Sof(C76)=
 Sof(H76A)=Sof(H76B)=Sof(C77)=Sof(H77A)=Sof(H77B)=FVAR(1)
 Sof(C21A)=Sof(H21D)=Sof(H21E)=Sof(H21F)=Sof(C22A)=Sof(H22D)=Sof(H22E)=
 Sof(H22F)=Sof(C23A)=Sof(H23D)=Sof(H23E)=Sof(H23F)=1-FVAR(2)
 Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=
 Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=FVAR(2)
7.a Ternary CH refined with riding coordinates:
 C30(H30), C33(H33), C36(H36), C45(H45), C48(H48), C51(H51)
7.b Secondary CH2 refined with riding coordinates:
 C54(H54A,H54B), C58(H58A,H58B), C62(H62A,H62B), C63(H63A,H63B), C64(H64A,
 H64B), C65(H65A,H65B), C66(H66A,H66B), C67(H67A,H67B), C68(H68A,H68B),
 C69(H69A,H69B), C70(H70A,H70B), C71(H71A,H71B), C72(H72A,H72B), C73(H73A,H73B),
  C74(H74A,H74B), C75(H75A,H75B), C76(H76A,H76B), C77(H77A,H77B), C74A(H74C,
 H74D), C75A(H75C,H75D), C76A(H76C,H76D), C77A(H77C,H77D)
7.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), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,
 H23B,H23C), C21A(H21D,H21E,H21F), C22A(H22D,H22E,H22F), C23A(H23D,H23E,H23F),
 C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C35(H35A,H35B,
 H35C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C46(H46A,H46B,H46C), 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), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C)
7.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C0AA(H0AA), C8(H8), C26(H26), C28(H28), C41(H41), C43(H43)
;
_shelx_res_checksum              67794
_shelx_fab_checksum              40696
_olex2_submission_special_instructions 'No special instructions were received'