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_7717414
_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         'C56 H69 N3 O2 P Sc'
_chemical_formula_sum            'C56 H69 N3 O2 P Sc'
_chemical_formula_weight         892.07
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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                 97.0520(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2105(4)
_cell_length_b                   23.0554(9)
_cell_length_c                   19.3556(7)
_cell_measurement_reflns_used    9885
_cell_measurement_temperature    119.99
_cell_measurement_theta_max      24.59
_cell_measurement_theta_min      2.30
_cell_volume                     4964.9(3)
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      119.99
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1215
_diffrn_reflns_av_unetI/netI     0.0754
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            83669
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.488
_diffrn_reflns_theta_min         2.032
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.224
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4657
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1146 before and 0.0950 after correction.
The Ratio of minimum to maximum transmission is 0.6246.
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    1.193
_exptl_crystal_description       block
_exptl_crystal_F_000             1912
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.372
_refine_diff_density_min         -0.505
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     583
_refine_ls_number_reflns         11378
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1030
_refine_ls_R_factor_gt           0.0497
_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^)+(0.0366P)^2^+4.6760P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1078
_refine_ls_wR_factor_ref         0.1405
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7350
_reflns_number_total             11378
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02838d2.cif
_cod_data_source_block           Complex_4_0ma_a
_cod_depositor_comments
'Adding full bibliography for 7717412--7717419.cif.'
_cod_database_code               7717414
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.971
_shelx_estimated_absorpt_t_min   0.965
_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:
 C46(H46), C5(H5), C3(H3), C4(H4), C47(H47), C53(H53), C49(H49), C17(H17),
 C35(H35), C42(H42), C34(H34), C48(H48), C41(H41), C36(H36), C19(H19), C43(H43),
  C40(H40), C18(H18), C44(H44), C54(H54), C56(H56), C55(H55), C37(H37), C38(H38)
2.b Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C14(H14A,H14B,H14C), C10(H10A,H10B,H10C), C13(H13A,H13B,
 H13C), C12(H12A,H12B,H12C), C31(H31A,H31B,H31C), C30(H30A,H30B,H30C), C9(H9A,
 H9B,H9C), C28(H28A,H28B,H28C), C26(H26A,H26B,H26C), C8(H8A,H8B,H8C), C22(H22A,
 H22B,H22C), C27(H27A,H27B,H27C), C24(H24A,H24B,H24C), C23(H23A,H23B,H23C)
;
_shelx_res_checksum              23323
_shelx_hkl_checksum              6203
_olex2_submission_special_instructions 'No special instructions were received'