A monoanionic pentadentate ligand platform for scandium-pnictogen multiple bonds.
Patrick, Evan A.; Yang, Yan; Piers, Warren E.; Maron, Laurent; Gelfand, Benjamin S.; Chemical communications (Cambridge, England) 57 (2021) 8640–8643; doi:10.1039/d1cc03481b

data_7128735
_publ_section_title
;
 A monoanionic pentadentate ligand platform for scandium-pnictogen
 multiple bonds.
;
_journal_issue                   69
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              8640
_journal_page_last               8643
_journal_paper_doi               10.1039/d1cc03481b
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C42 H44 B N7 P Sc, C5 H12'
_chemical_formula_sum            'C47 H56 B N7 P Sc'
_chemical_formula_weight         805.72
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-04-28
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-06-16 deposited with the CCDC.	2021-08-03 downloaded from the CCDC.
;
_cell_angle_alpha                93.476(6)
_cell_angle_beta                 95.859(7)
_cell_angle_gamma                91.758(6)
_cell_formula_units_Z            2
_cell_length_a                   8.3970(18)
_cell_length_b                   10.808(2)
_cell_length_c                   24.445(5)
_cell_measurement_reflns_used    3485
_cell_measurement_temperature    173.0
_cell_measurement_theta_max      66.695
_cell_measurement_theta_min      19.895
_cell_volume                     2201.3(8)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            29561
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        66.595
_diffrn_reflns_theta_max         66.595
_diffrn_reflns_theta_min         1.820
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           0.64
_diffrn_source_power             0.0285952
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           44.68
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.080
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.5947
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0795 before and 0.0226 after correction.
The Ratio of minimum to maximum transmission is 0.7900.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_description       plank
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.424
_exptl_crystal_size_mid          0.182
_exptl_crystal_size_min          0.056
_refine_diff_density_max         0.357
_refine_diff_density_min         -0.302
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     698
_refine_ls_number_reflns         7754
_refine_ls_number_restraints     1123
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0359
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0497P)^2^+0.9020P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.0962
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7397
_reflns_number_total             7754
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc03481b2.cif
_cod_data_source_block           ep538
_cod_depositor_comments
'Adding full bibliography for 7128734--7128737.cif.'
_cod_original_cell_volume        2201.4(8)
_cod_database_code               7128735
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.892
_shelx_estimated_absorpt_t_min   0.473
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H12-H15A = H12-H15B
 -2.3 with sigma of 0.02
 C1S_1-C2S_1 \\sim C2S_1-C3S_1 \\sim C3S_1-C4S_1 \\sim C4S_1-C5S_1
 C1S_2-C2S_2 \\sim C2S_2-C3S_2 \\sim C3S_2-C4S_2 \\sim C4S_2-C5S_2
 with sigma of 0.02
 C1S_1-C3S_1 \\sim C2S_1-C4S_1 \\sim C3S_1-C5S_1
 C1S_2-C3S_2 \\sim C2S_2-C4S_2 \\sim C3S_2-C5S_2
 with sigma of 0.04
 Sc1-N6B \\sim Sc1-N6A
 with sigma of 0.02
 C32-C37A \\sim C32-C37B \\sim C32-C39A \\sim C32-C39B
 with sigma of 0.04
 C37A-C39A \\sim C37B-C39B
 with sigma of 0.04
 C38-C37A \\sim C39A-C38 \\sim C38-C37B \\sim C39B-C38
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C3S_2 \\sim C1S_2 \\sim C2S_2 \\sim C4S_2 \\sim C5S_2 \\sim C3S_1 \\sim C1S_1
\\sim C2S_1 \\sim C4S_1 \\sim C5S_1: within 3A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 3A
C37A \\sim C39A \\sim C39B \\sim C37B: within 1A with sigma of 0.003 and sigma
for terminal atoms of 0.003 within 1A
N6A \\sim C19A \\sim C20A \\sim C21A \\sim C22A \\sim C23A \\sim C24A \\sim
C25A \\sim N6B \\sim C19B \\sim C20B \\sim C21B \\sim C22B \\sim C23B \\sim
C24B \\sim C25B \\sim C15B \\sim C16B \\sim C17B \\sim C18B \\sim C15A \\sim
C16A \\sim C17A \\sim C18A: within 3A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 3A
4. Same fragment restrains
{N6A, C15A, C16A, C17A, C18A, C19A, C20A, C21A, C22A, C23A, C24A, C25A} sigma
for 1-2: 0.04, 1-3: 0.06
as in
{N6B, C15B, C16B, C17B, C18B, C19B, C20B, C21B, C22B, C23B, C24B, C25B}
5. Others
 Sof(C1S)=Sof(H1SA)=Sof(H1SB)=Sof(H1SC)=Sof(C2S)=Sof(H2SA)=Sof(H2SB)=Sof(C3S)=
 Sof(H3SA)=Sof(H3SB)=Sof(C4S)=Sof(H4SA)=Sof(H4SB)=Sof(C5S)=Sof(H5SA)=Sof(H5SB)=
 Sof(H5SC)=1-FVAR(1)
 Sof(C1S)=Sof(H1SA)=Sof(H1SB)=Sof(H1SC)=Sof(C2S)=Sof(H2SA)=Sof(H2SB)=Sof(C3S)=
 Sof(H3SA)=Sof(H3SB)=Sof(C4S)=Sof(H4SA)=Sof(H4SB)=Sof(C5S)=Sof(H5SA)=Sof(H5SB)=
 Sof(H5SC)=FVAR(1)
 Sof(N6B)=Sof(C19B)=Sof(C20B)=Sof(H20D)=Sof(H20E)=Sof(H20F)=Sof(C21B)=
 Sof(C22B)=Sof(H22B)=Sof(C23B)=Sof(H23B)=Sof(C24B)=Sof(H24B)=Sof(C25B)=
 Sof(H25B)=1-FVAR(2)
 Sof(N6A)=Sof(C19A)=Sof(C20A)=Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(C21A)=
 Sof(C22A)=Sof(H22A)=Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(H24A)=Sof(C25A)=
 Sof(H25A)=FVAR(2)
 Sof(H13D)=Sof(H13E)=Sof(H13F)=1-FVAR(3)
 Sof(H13A)=Sof(H13B)=Sof(H13C)=FVAR(3)
 Sof(H38A)=Sof(C39B)=Sof(H39D)=Sof(H39E)=Sof(H39F)=Sof(C37B)=Sof(H37D)=
 Sof(H37E)=Sof(H37F)=1-FVAR(4)
 Sof(C37A)=Sof(H37A)=Sof(H37B)=Sof(H37C)=Sof(H38)=Sof(C39A)=Sof(H39A)=
 Sof(H39B)=Sof(H39C)=FVAR(4)
 Sof(C15B)=Sof(H15B)=Sof(C16B)=Sof(H16B)=Sof(C17B)=Sof(H17B)=Sof(C18B)=1-FVAR(5)
 Sof(C15A)=Sof(H15A)=Sof(C16A)=Sof(H16A)=Sof(C17A)=Sof(H17A)=Sof(C18A)=FVAR(5)
6.a Ternary CH refined with riding coordinates:
 C38(H38), C38(H38A), C41(H41)
6.b Secondary CH2 refined with riding coordinates:
 C2S(H2SA,H2SB), C3S(H3SA,H3SB), C4S(H4SA,H4SB), C2S(H2SA,H2SB), C3S(H3SA,
 H3SB), C4S(H4SA,H4SB)
6.c Me refined with riding coordinates:
 C1S(H1SA,H1SB,H1SC), C5S(H5SA,H5SB,H5SC), C1S(H1SA,H1SB,H1SC), C5S(H5SA,H5SB,
 H5SC)
6.d Aromatic/amide H refined with riding coordinates:
 C15A(H15A), C16A(H16A), C17A(H17A), C22A(H22A), C23A(H23A), C24A(H24A),
 C25A(H25A), C15B(H15B), C16B(H16B), C17B(H17B), C22B(H22B), C23B(H23B),
 C24B(H24B), C25B(H25B), C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8),
  C9(H9), C11(H11), C12(H12), C27(H27), C28(H28), C29(H29), C30(H30), C33(H33),
 C34(H34), C35(H35)
6.e Disordered Me refined with riding coordinates:
 C13(H13A,H13B,H13C,H13D,H13E,H13F)
6.f Idealised Me refined as rotating group:
 C20A(H20A,H20B,H20C), C20B(H20D,H20E,H20F), C37A(H37A,H37B,H37C), C39A(H39A,
 H39B,H39C), C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C39B(H39D,H39E,H39F),
 C37B(H37D,H37E,H37F)
;
_shelx_res_checksum              42478
_shelx_hkl_checksum              36033
_olex2_submission_special_instructions 'No special instructions were received'