Generation and reactivity of neutral 1,3-benzazaphosphole and anionic 1,3-benzazaphospholide ytterbium(iii) complexes.
Ying, Huacheng; Gong, Mingzhu; Pi, Chengfu; Dalton transactions (Cambridge, England : 2003) 48 (2019) 2722–2729; doi:10.1039/c8dt04768e

data_7048776
_publ_section_title
;
 Generation and reactivity of neutral 1,3-benzazaphosphole and anionic
 1,3-benzazaphospholide ytterbium(iii) complexes.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2722
_journal_page_last               2729
_journal_paper_doi               10.1039/c8dt04768e
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C24 H21 N P Yb, C15 H15 Yb'
_chemical_formula_sum            'C39 H36 N P Yb2'
_chemical_formula_weight         895.74
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-01-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-01-09 deposited with the CCDC.
2019-01-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.923(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   38.220(6)
_cell_length_b                   8.3463(14)
_cell_length_c                   22.987(4)
_cell_measurement_reflns_used    4675
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      26.326
_cell_measurement_theta_min      2.370
_cell_volume                     6594.9(19)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0626
_diffrn_reflns_av_unetI/netI     0.0762
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            15566
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.024
_diffrn_reflns_theta_max         25.024
_diffrn_reflns_theta_min         2.511
_exptl_absorpt_coefficient_mu    5.714
_exptl_absorpt_correction_T_max  0.8729
_exptl_absorpt_correction_T_min  0.5610
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
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_exptl_crystal_description       prism
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_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.639
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         5785
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0805
_refine_ls_R_factor_gt           0.0562
_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^)+(0.0794P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1327
_refine_ls_wR_factor_ref         0.1445
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4305
_reflns_number_total             5785
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04768e2.cif
_cod_data_source_block           4b
_cod_depositor_comments
'Adding full bibliography for 7048775--7048777.cif.'
_cod_original_cell_volume        6594.8(19)
_cod_database_code               7048776
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.726
_shelx_estimated_absorpt_t_min   0.481
_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 body (RIGU) restrains
 C35, C36, C37, C38, C39, C34, C33, C32, C31, C30
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Ternary CH refined with riding coordinates:
 C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23),
 C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31),
  C32(H32), C33(H33), C35(H35), C38(H38), C39(H39)
3.b Me refined with riding coordinates:
 C7(H7A,H7B,H7C)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C34(H34), C36(H36), C37(H37)
;
_shelx_res_checksum              28103
_olex2_submission_special_instructions 'No special instructions were received'