Reactions of a geminal Sc/P Lewis pair with pyridotetrazole and beyond.
Guan, Yiwen; Xu, Xian; Xu, Xin; Dalton transactions (Cambridge, England : 2003) 54 (2024) 222–230; doi:10.1039/d4dt02838d

data_7717419
_publ_section_title
;
 Reactions of a geminal Sc/P Lewis pair with pyridotetrazole and beyond.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              222
_journal_page_last               230
_journal_paper_doi               10.1039/d4dt02838d
_journal_volume                  54
_journal_year                    2024
_chemical_formula_moiety         'C91 H125 N5 O4 P2 Sc2'
_chemical_formula_sum            'C91 H125 N5 O4 P2 Sc2'
_chemical_formula_weight         1504.81
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-10-08
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-10-09 deposited with the CCDC.	2024-11-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.566(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.380(7)
_cell_length_b                   12.984(3)
_cell_length_c                   29.626(7)
_cell_measurement_reflns_used    9534
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      59.688
_cell_measurement_theta_min      2.647
_cell_volume                     8949(4)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.1543
_diffrn_reflns_av_unetI/netI     0.0887
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            115648
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        52.982
_diffrn_reflns_theta_max         52.982
_diffrn_reflns_theta_min         2.647
_diffrn_source_current           3.57
_diffrn_source_power             0.24947159999999996
_diffrn_source_voltage           69.88
_exptl_absorpt_coefficient_mu    1.345
_exptl_absorpt_correction_T_max  0.7518
_exptl_absorpt_correction_T_min  0.4742
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1756 before and 0.1027 after correction.
The Ratio of minimum to maximum transmission is 0.6308.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.117
_exptl_crystal_description       block
_exptl_crystal_F_000             3240
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.645
_refine_diff_density_min         -0.783
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     969
_refine_ls_number_reflns         15791
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0959
_refine_ls_R_factor_gt           0.0786
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1446P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2115
_refine_ls_wR_factor_ref         0.2258
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11936
_reflns_number_total             15791
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02838d2.cif
_cod_data_source_block           Complex_3_0m_a
_cod_depositor_comments
'Adding full bibliography for 7717412--7717419.cif.'
_cod_database_code               7717419
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.948
_shelx_estimated_absorpt_t_min   0.877
_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 Ternary CH refined with riding coordinates:
 C45(H45)
2.b Aromatic/amide H refined with riding coordinates:
 C46(H46), C47(H47), C44(H44), C81(H81), C87(H87), C38(H38), C66(H66),
 C64(H64), C91(H91), C3(H3), C90(H90), C52(H52), C50(H50), C65(H65), C40(H40),
 C51(H51), C88(H88), C19(H19), C89(H89), C37(H37), C42(H42), C34(H34), C85(H85),
  C82(H82), C43(H43), C5(H5), C4(H4), C17(H17), C41(H41), C36(H36), C18(H18),
 C83(H83), C35(H35), C84(H84)
2.c Idealised Me refined as rotating group:
 C79(H79A,H79B,H79C), C56(H56A,H56B,H56C), C75(H75A,H75B,H75C), C71(H71A,H71B,
 H71C), C78(H78A,H78B,H78C), C22(H22A,H22B,H22C), C61(H61A,H61B,H61C), C69(H69A,
 H69B,H69C), C74(H74A,H74B,H74C), C55(H55A,H55B,H55C), C77(H77A,H77B,H77C),
 C24(H24A,H24B,H24C), C60(H60A,H60B,H60C), C30(H30A,H30B,H30C), C59(H59A,H59B,
 H59C), C70(H70A,H70B,H70C), C73(H73A,H73B,H73C), C57(H57A,H57B,H57C), C31(H31A,
 H31B,H31C), C23(H23A,H23B,H23C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C8(H8A,
 H8B,H8C), C28(H28A,H28B,H28C), C27(H27A,H27B,H27C), C13(H13A,H13B,H13C),
 C32(H32A,H32B,H32C), C14(H14A,H14B,H14C), C26(H26A,H26B,H26C), C12(H12A,H12B,
 H12C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              46280
_shelx_hkl_checksum              87667
_shelx_fab_checksum              85822
_olex2_submission_special_instructions 'No special instructions were received'