N-Heterocyclic carbene phosphaketene adducts as precursors to carbene-phosphinidene adducts and a rearranged π-system.
Li, Zhongshu; Chen, Xiaodan; Li, Yaqi; Su, Cheng-Yong; Grützmacher, Hansjörg; Chemical communications (Cambridge, England) 52 (2016) 11343–11346; doi:10.1039/c6cc05916c

data_7124962
_publ_section_title
;
 N-Heterocyclic carbene phosphaketene adducts as precursors to
 carbene-phosphinidene adducts and a rearranged \p-system.
;
_journal_issue                   76
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              11343
_journal_page_last               11346
_journal_paper_doi               10.1039/c6cc05916c
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C46 H51 Ge N2 O P'
_chemical_formula_sum            'C46 H51 Ge N2 O P'
_chemical_formula_weight         751.44
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_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
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Olex2 1.2
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2016-03-18 deposited with the CCDC.
2016-08-09 downloaded from the CCDC.
;
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
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_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
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_diffrn_measurement_details
;
  1 omega  -30.00   70.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       -0.9338   77.0000 -120.0000 100

  2 omega  -84.00  -35.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       -0.9338 -178.0000    0.0000 49

  3 omega    8.00  109.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       87.6717  -95.0000   30.0000 101

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omega____ theta____ kappa____ phi______ frames
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  5 omega   25.00   98.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
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  6 omega    9.00  128.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
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  7 omega   24.00   90.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
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  8 omega   76.00  152.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       87.6717   45.0000 -150.0000 76

  9 omega   16.00  118.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       87.6717  -77.0000 -120.0000 102
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
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_diffrn_orient_matrix_UB_22      0.0697327000
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_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
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_diffrn_reflns_av_unetI/netI     0.0147
_diffrn_reflns_Laue_measured_fraction_full 0.930
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_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20983
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_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         65.369
_diffrn_reflns_theta_min         3.726
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.661
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71666
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_F_000             1584
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_refine_diff_density_max         0.440
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_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_gt           0.0251
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0355P)^2^+2.1496P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0664
_refine_ls_wR_factor_ref         0.0678
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6414
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_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc05916c2.cif
_cod_data_source_block           exp_1998
_cod_original_cell_volume        4067.62(5)
_cod_database_code               7124962
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_chemical_oxdiff_formula         'C H N O P Ge'
_reflns_odcompleteness_completeness 99.80
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_olex2_refinement_description
;
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_olex2_date_sample_data_collection 2015-06-27
_olex2_submission_special_instructions 'No special instructions were received'