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_7048777
_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         'C41 H19 B F15 N P Yb, C7 H8'
_chemical_formula_sum            'C48 H27 B F15 N P Yb'
_chemical_formula_weight         1117.52
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-01-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-01-17 deposited with the CCDC.
2019-01-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.1000(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.2386(6)
_cell_length_b                   21.6434(10)
_cell_length_c                   15.4959(7)
_cell_measurement_reflns_used    9888
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      27.619
_cell_measurement_theta_min      2.453
_cell_volume                     4341.4(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.964
_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  0.0232
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25978
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.637
_diffrn_reflns_theta_min         2.461
_exptl_absorpt_coefficient_mu    2.292
_exptl_absorpt_correction_T_max  0.8917
_exptl_absorpt_correction_T_min  0.6652
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.710
_exptl_crystal_description       block
_exptl_crystal_F_000             2188
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.872
_refine_diff_density_min         -0.690
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     605
_refine_ls_number_reflns         9750
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0264
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0249P)^2^+6.3850P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0604
_refine_ls_wR_factor_ref         0.0645
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8159
_reflns_number_total             9750
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04768e2.cif
_cod_data_source_block           5c
_cod_depositor_comments
'Adding full bibliography for 7048775--7048777.cif.'
_cod_database_code               7048777
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.894
_shelx_estimated_absorpt_t_min   0.787
_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:
 C36(H36), C35(H35), C34(H34), C33(H33), C32(H32), C38(H38), C39(H39),
 C40(H40), C41(H41), C37(H37), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31),
  C4(H4), C5(H5), C6(H6), C7(H7), C42(H42), C43(H43), C44(H44), C45(H45),
 C46(H46)
2.b Idealised Me refined as rotating group:
 C48(H48A,H48B,H48C)
;
_shelx_res_checksum              92840
_olex2_submission_special_instructions 'No special instructions were received'