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_7128737
_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         'C44 H44 B N7 O4 P Sc, 2(C3 H3)'
_chemical_formula_sum            'C50 H50 B N7 O4 P Sc'
_chemical_formula_weight         899.71
_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             2021-06-07
_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                90.965(3)
_cell_angle_beta                 91.117(3)
_cell_angle_gamma                101.418(2)
_cell_formula_units_Z            2
_cell_length_a                   8.7025(3)
_cell_length_b                   12.7011(4)
_cell_length_c                   21.2188(10)
_cell_measurement_reflns_used    9863
_cell_measurement_temperature    173.0
_cell_measurement_theta_max      72.380
_cell_measurement_theta_min      3.551
_cell_volume                     2297.98(15)
_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 2018/2 (Sheldrick, 2018)'
_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 0.963
_diffrn_measured_fraction_theta_max 0.963
_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  0.0621
_diffrn_reflns_av_unetI/netI     0.0718
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            26336
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        66.594
_diffrn_reflns_theta_max         66.594
_diffrn_reflns_theta_min         2.083
_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    2.122
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.6488
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0805 before and 0.0602 after correction.
The Ratio of minimum to maximum transmission is 0.8609.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_description       rod
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.221
_exptl_crystal_size_mid          0.065
_exptl_crystal_size_min          0.059
_refine_diff_density_max         0.536
_refine_diff_density_min         -0.360
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     726
_refine_ls_number_reflns         7812
_refine_ls_number_restraints     1276
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0528
_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^)+(0.0468P)^2^+1.5860P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1284
_refine_ls_wR_factor_ref         0.1355
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6405
_reflns_number_total             7812
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc03481b2.cif
_cod_data_source_block           ep-555
_cod_depositor_comments
'Adding full bibliography for 7128734--7128737.cif.'
_cod_database_code               7128737
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.885
_shelx_estimated_absorpt_t_min   0.651
_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. Restrained distances
 P1-C28 \\sim P1-C28A
 with sigma of 0.02
 P1-C33A \\sim P1-C33
 with sigma of 0.02
3. Restrained planarity
 P1, N7, C28, C29, C30, C31, C32
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
N7 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim N7A \\sim C32A \\sim
C31A \\sim C30A \\sim C29A \\sim C28A \\sim C33 \\sim C34 \\sim C35 \\sim C36
\\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41 \\sim C42 \\sim C43 \\sim C44
\\sim C33A \\sim C34A \\sim C35A \\sim C36A \\sim C37A \\sim C38A \\sim C39A
\\sim C40A \\sim C41A \\sim C42A \\sim C43A \\sim C44A: within 3A with sigma of
0.02 and sigma for terminal atoms of 0.04 within 3A
5. Same fragment restrains
{N7, C28, C29, C30, C31, C32} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N7A, C32A, C31A, C30A, C29A, C28A}
{C33, C34, C35, C36, C37, C38, C39, C40, C41, C42, C43, C44} sigma for 1-2:
0.02, 1-3: 0.04
as in
{C33A, C34A, C35A, C36A, C37A, C38A, C39A, C40A, C41A, C42A, C43A, C44A}
6. Others
 Sof(N7A)=Sof(C32A)=Sof(H32A)=Sof(C31A)=Sof(H31A)=Sof(C30A)=Sof(H30A)=
 Sof(C29A)=Sof(H29A)=Sof(C28A)=Sof(C33A)=Sof(C34A)=Sof(C35A)=Sof(H35A)=
 Sof(C36A)=Sof(H36A)=Sof(C37A)=Sof(H37A)=Sof(C38A)=Sof(C39A)=Sof(H39D)=
 Sof(H39E)=Sof(H39F)=Sof(C40A)=Sof(H40A)=Sof(C41A)=Sof(H41D)=Sof(H41E)=
 Sof(H41F)=Sof(C42A)=Sof(H42D)=Sof(H42E)=Sof(H42F)=Sof(C43A)=Sof(H43A)=
 Sof(C44A)=Sof(H44D)=Sof(H44E)=Sof(H44F)=1-FVAR(1)
 Sof(N7)=Sof(C28)=Sof(C29)=Sof(H29)=Sof(C30)=Sof(H30)=Sof(C31)=Sof(H31)=
 Sof(C32)=Sof(H32)=Sof(C33)=Sof(C34)=Sof(C35)=Sof(H35)=Sof(C36)=Sof(H36)=
 Sof(C37)=Sof(H37)=Sof(C38)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=Sof(C40)=
 Sof(H40)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H41C)=Sof(C42)=Sof(H42A)=Sof(H42B)=
 Sof(H42C)=Sof(C43)=Sof(H43)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(H44C)=FVAR(1)
7.a Ternary CH refined with riding coordinates:
 C40(H40), C43(H43), C40A(H40A), C43A(H43A)
7.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C11(H11),
 C12(H12), C15(H15), C16(H16), C17(H17), C22(H22), C23(H23), C24(H24), C25(H25),
  C29(H29), C30(H30), C31(H31), C32(H32), C32A(H32A), C31A(H31A), C30A(H30A),
 C29A(H29A), C35(H35), C36(H36), C37(H37), C35A(H35A), C36A(H36A), C37A(H37A),
 C1S(H1S), C2S(H2S), C3S(H3S), C4S(H4S), C5S(H5S), C6S(H6S)
7.c Fitted hexagon refined as free rotating group:
 C33(C34,C35,C36,C37,C38), C33A(C34A,C35A,C36A,C37A,C38A)
7.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C20(H20A,H20B,H20C), C39(H39A,H39B,H39C), C41(H41A,H41B,
 H41C), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C), C39A(H39D,H39E,H39F),
 C41A(H41D,H41E,H41F), C42A(H42D,H42E,H42F), C44A(H44D,H44E,H44F)
;
_shelx_res_checksum              88152
_shelx_hkl_checksum              17281
_olex2_submission_special_instructions 'No special instructions were received'