CO reductive oligomerization by a divalent thulium complex and CO2-induced functionalization
Simler, Thomas; McCabe, Karl Nael; Maron, Laurent; Nocton, Grégory; Chemical Science  (2022) –; doi:10.1039/D2SC01798A

data_1566943
_publ_section_title
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 CO reductive oligomerization by a divalent thulium complex and
 CO2-induced functionalization
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC01798A
_journal_year                    2022
_chemical_formula_moiety         'C109 H177 O6 Tm3'
_chemical_formula_sum            'C109 H177 O6 Tm3'
_chemical_formula_weight         2090.29
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-09-07
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6394)
;
_cell_angle_alpha                90
_cell_angle_beta                 105.969(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   29.457(2)
_cell_length_b                   16.1306(12)
_cell_length_c                   46.333(4)
_cell_measurement_reflns_used    9837
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      25.873
_cell_measurement_theta_min      2.176
_cell_volume                     21166(3)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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  0.0858
_diffrn_reflns_av_unetI/netI     0.0635
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       60
_diffrn_reflns_limit_l_min       -60
_diffrn_reflns_number            142322
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.556
_diffrn_reflns_theta_min         1.608
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.542
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6786
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0974 before and 0.0572 after correction.
The Ratio of minimum to maximum transmission is 0.9101.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_description       plate
_exptl_crystal_F_000             8688
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.382
_refine_diff_density_min         -1.874
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1118
_refine_ls_number_reflns         24372
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0366
_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^)+(0.0164P)^2^+93.6164P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0674
_refine_ls_wR_factor_ref         0.0784
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17506
_reflns_number_total             24372
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc01798a4.cif
_cod_data_source_block           6
_cod_database_code               1566943
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.905
_shelx_estimated_absorpt_t_min   0.750
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C11(H11), C27(H27), C29(H29), C44(H44), C46(H46), C61(H61), C63(H63),
 C78(H78), C80(H80), C95(H95), C97(H97)
2.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C22(H22A,
 H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C31(H31A,H31B,H31C),
 C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C35(H35A,H35B,H35C), C36(H36A,H36B,
 H36C), C37(H37A,H37B,H37C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C41(H41A,
 H41B,H41C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C),
 C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C56(H56A,H56B,
 H56C), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C), C65(H65A,H65B,H65C), C66(H66A,
 H66B,H66C), C67(H67A,H67B,H67C), C69(H69A,H69B,H69C), C70(H70A,H70B,H70C),
 C71(H71A,H71B,H71C), C73(H73A,H73B,H73C), C74(H74A,H74B,H74C), C75(H75A,H75B,
 H75C), C82(H82A,H82B,H82C), C83(H83A,H83B,H83C), C84(H84A,H84B,H84C), C86(H86A,
 H86B,H86C), C87(H87A,H87B,H87C), C88(H88A,H88B,H88C), C90(H90A,H90B,H90C),
 C91(H91A,H91B,H91C), C92(H92A,H92B,H92C), C99(H99A,H99B,H99C), C100(H10A,H10B,
 H10C), C101(H10D,H10E,H10F), C103(H10G,H10H,H10I), C104(H10J,H10K,H10L),
 C105(H10M,H10N,H10O), C107(H10P,H10Q,H10R), C108(H10S,H10T,H10U), C109(H10V,
 H10W,H10X)
;
_shelx_res_checksum              93703
_shelx_hkl_checksum              70882
_olex2_submission_special_instructions 'No special instructions were received'