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_7048775
_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         '2(C15 H15 Yb), 2(C17 H18 N P), C7 H8'
_chemical_formula_sum            'C71 H74 N2 P2 Yb2'
_chemical_formula_weight         1363.34
_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
_audit_creation_date             2019-01-03
_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                 96.515(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.082(2)
_cell_length_b                   14.797(2)
_cell_length_c                   25.996(4)
_cell_measurement_reflns_used    9835
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.455
_cell_measurement_theta_min      2.356
_cell_volume                     6146.2(15)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_collection       '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 0.998
_diffrn_measured_fraction_theta_max 0.995
_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  0.0611
_diffrn_reflns_av_unetI/netI     0.0583
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            55943
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.493
_diffrn_reflns_theta_min         1.876
_exptl_absorpt_coefficient_mu    3.119
_exptl_absorpt_correction_T_max  0.6192
_exptl_absorpt_correction_T_min  0.5887
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2736
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.381
_refine_diff_density_min         -1.263
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     740
_refine_ls_number_reflns         14043
_refine_ls_number_restraints     80
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0408
_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^)+(0.0472P)^2^+5.3228P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1001
_refine_ls_wR_factor_ref         0.1062
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11156
_reflns_number_total             14043
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04768e2.cif
_cod_data_source_block           2a
_cod_depositor_comments
'Adding full bibliography for 7048775--7048777.cif.'
_cod_original_cell_volume        6146.1(16)
_cod_database_code               7048775
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.619
_shelx_estimated_absorpt_t_min   0.589
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 C43A, C41, C42, C42A, C43, C40A, C41A, C44, C44A, C40, Yb2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Others
 Sof(C40A)=Sof(H40A)=Sof(C41A)=Sof(H41A)=Sof(C42A)=Sof(H42A)=Sof(C43A)=
 Sof(H43A)=Sof(C44A)=Sof(H44A)=1-FVAR(1)
 Sof(C40)=Sof(H40)=Sof(C41)=Sof(H41)=Sof(C42)=Sof(H42)=Sof(C43)=Sof(H43)=
 Sof(C44)=Sof(H44)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C36(H36), C38(H38), C42(H42), C43(H43), C43A(H43A), C45(H45), C46(H46),
 C47(H47), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C58(H58), C59(H59),
  C60(H60), C61(H61), C62(H62), C63(H63)
4.b Me refined with riding coordinates:
 C7(H7A,H7B,H7C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,
 H17C), C24(H24A,H24B,H24C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,
 H34B,H34C), C71(H71A,H71B,H71C)
4.c Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2A), C2(H2), C4(H4), C5(H5), C11(H11), C13(H13), C19(H19),
 C21(H21), C22(H22), C27(H27), C29(H29), C35(H35), C37(H37), C39(H39), C40(H40),
  C40A(H40A), C41(H41), C41A(H41A), C42A(H42A), C44(H44), C44A(H44A), C48(H48),
 C49(H49), C50(H50), C51(H51), C57(H57), C64(H64), C65(H65), C66(H66), C67(H67),
  C69(H69), C70(H70)
;
_shelx_res_checksum              75896
_olex2_submission_special_instructions 'No special instructions were received'