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_7717416
_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         'C47 H70 N2 O2 P Sc Si'
_chemical_formula_sum            'C47 H70 N2 O2 P Sc Si'
_chemical_formula_weight         799.07
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/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                 102.852(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   41.237(4)
_cell_length_b                   10.5045(10)
_cell_length_c                   21.735(2)
_cell_measurement_reflns_used    9487
_cell_measurement_temperature    153
_cell_measurement_theta_max      23.79
_cell_measurement_theta_min      2.27
_cell_volume                     9179.2(15)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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      153
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.1396
_diffrn_reflns_av_unetI/netI     0.1214
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       53
_diffrn_reflns_limit_h_min       -53
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            66916
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.509
_diffrn_reflns_theta_min         2.271
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.259
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6941
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1855 before and 0.0819 after correction.
The Ratio of minimum to maximum transmission is 0.9311.
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    1.156
_exptl_crystal_description       block
_exptl_crystal_F_000             3456
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.540
_refine_diff_density_min         -0.420
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         10545
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.1504
_refine_ls_R_factor_gt           0.0627
_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^)+(0.0460P)^2^+10.7379P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1113
_refine_ls_wR_factor_ref         0.1349
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5811
_reflns_number_total             10545
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02838d2.cif
_cod_data_source_block           Complex_8_0ma_a
_cod_depositor_comments
'Adding full bibliography for 7717412--7717419.cif.'
_cod_original_cell_volume        9179.1(15)
_cod_database_code               7717416
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.962
_shelx_estimated_absorpt_t_min   0.955
_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. Rigid bond restraints
 C32, C29
 with sigma for 1-2 distances of 0.0002 and sigma for 1-3 distances of 0.0001
 C30, C29
 with sigma for 1-2 distances of 0.0002 and sigma for 1-3 distances of 0.0001
 C29, C31
 with sigma for 1-2 distances of 0.0002 and sigma for 1-3 distances of 0.0001
 C29, N1
 with sigma for 1-2 distances of 0.0002 and sigma for 1-3 distances of 0.0001
3.a Aromatic/amide H refined with riding coordinates:
 C19(H19), C41(H41), C37(H37), C43(H43), C3(H3), C17(H17), C47(H47), C39(H39),
 C40(H40), C18(H18), C38(H38), C44(H44), C5(H5), C4(H4), C45(H45), C46(H46)
3.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C26(H26A,H26B,H26C), C31(H31A,H31B,H31C), C28(H28A,H28B,
 H28C), C9(H9A,H9B,H9C), C32(H32A,H32B,H32C), C10(H10A,H10B,H10C), C27(H27A,
 H27B,H27C), C34(H34A,H34B,H34C), C33(H33A,H33B,H33C), C30(H30A,H30B,H30C),
 C22(H22A,H22B,H22C), C35(H35A,H35B,H35C), C23(H23A,H23B,H23C), C12(H12A,H12B,
 H12C), C13(H13A,H13B,H13C), C24(H24A,H24B,H24C), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              34444
_shelx_hkl_checksum              85180
_olex2_submission_special_instructions 'No special instructions were received'