Nonbenzenoid aromaticity of 1-phosphafulvenes: synthesis of phosphacymantrenes.
Liu, Yanjie; Tian, Rongqiang; Duan, Zheng; Mathey, François; Dalton transactions (Cambridge, England : 2003) 50 (2021) 476–479; doi:10.1039/d0dt03934a

data_7706038
_publ_section_title
;
 Nonbenzenoid aromaticity of 1-phosphafulvenes: synthesis of
 phosphacymantrenes.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              476
_journal_page_last               479
_journal_paper_doi               10.1039/d0dt03934a
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C42 H32 Mn2 N2 O6 P2, H2 O'
_chemical_formula_sum            'C42 H34 Mn2 N2 O7 P2'
_chemical_formula_weight         850.53
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
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Olex2 1.2
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2020-08-05 deposited with the CCDC.	2020-12-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.0866(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_length_c                   15.3780(2)
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_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
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;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      293(2)
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_diffrn_measurement_details
;
  1 omega  -11.00   15.00   1.0000    2.2500
omega____ theta____ kappa____ phi______ frames
    -      -33.5000   37.0000  150.0000 26

  2 omega -102.00  -33.00   1.0000    2.2500
omega____ theta____ kappa____ phi______ frames
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  3 omega -101.00  -22.00   1.0000    2.2500
omega____ theta____ kappa____ phi______ frames
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  4 omega   61.00   87.00   1.0000    2.2500
omega____ theta____ kappa____ phi______ frames
    -       36.4734   77.0000  -90.0000 26

  5 omega    8.00   83.00   1.0000    2.2500
omega____ theta____ kappa____ phi______ frames
    -       36.4734 -110.0000   60.0000 75

  6 omega   26.00   59.00   1.0000    2.2500
omega____ theta____ kappa____ phi______ frames
    -       36.4734   37.0000   30.0000 33

  7 omega   28.00   60.00   1.0000    2.2500
omega____ theta____ kappa____ phi______ frames
    -       36.4734   77.0000  -90.0000 32

  8 omega   73.00  110.00   1.0000    2.2500
omega____ theta____ kappa____ phi______ frames
    -       36.4734  178.0000 -150.0000 37

  9 omega   51.00  106.00   1.0000    2.2500
omega____ theta____ kappa____ phi______ frames
    -       36.4734   77.0000   30.0000 55

 10 omega   38.00   69.00   1.0000    2.2500
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -99.0000  -90.0000 31

 11 omega   66.00   92.00   1.0000    2.2500
omega____ theta____ kappa____ phi______ frames
    -       36.4734   37.0000   30.0000 26

 12 omega   12.00   53.00   1.0000    2.2500
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -57.0000 -180.0000 41

 13 omega   79.00  136.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000    0.0000 57

 14 omega   82.00  111.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000  120.0000 29

 15 omega   95.00  177.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000 -150.0000 82

 16 omega  108.00  173.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000   90.0000 65

 17 omega   38.00   63.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000  120.0000 25

 18 omega   99.00  173.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000 -120.0000 74

 19 omega   48.00   90.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   90.0000 42

 20 omega   37.00   63.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -150.0000 26

 21 omega   37.00  114.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000  -30.0000 77

 22 omega   40.00  109.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -61.0000  -60.0000 69
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
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_diffrn_orient_matrix_UB_11      0.0242336000
_diffrn_orient_matrix_UB_12      0.1058531000
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_diffrn_orient_matrix_UB_21      -0.0772474000
_diffrn_orient_matrix_UB_22      0.0344058000
_diffrn_orient_matrix_UB_23      0.0069192000
_diffrn_orient_matrix_UB_31      0.0173176000
_diffrn_orient_matrix_UB_32      0.0049996000
_diffrn_orient_matrix_UB_33      0.1005222000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_unetI/netI     0.0407
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            17079
_diffrn_reflns_point_group_measured_fraction_full 0.999
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_diffrn_reflns_theta_full        67.080
_diffrn_reflns_theta_max         67.080
_diffrn_reflns_theta_min         3.984
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.395
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_exptl_absorpt_correction_T_min  0.71074
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_description       prism
_exptl_crystal_F_000             1744
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_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
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_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
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_refine_ls_number_reflns         7061
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_refine_ls_R_factor_all          0.0534
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0518P)^2^+1.5169P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_reflns_number_gt                5817
_reflns_number_total             7061
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03934a2.cif
_cod_data_source_block           20170588
_cod_depositor_comments
'Adding full bibliography for 7706035--7706039.cif.'
_cod_original_cell_volume        3954.81(11)
_cod_database_code               7706038
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C38H70N2O2P2Mn1
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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, All O(H,H) groups
2.a Free rotating group:
 O7(H7A,H7B)
2.b Ternary CH refined with riding coordinates:
 C36(H36), C37(H37)
2.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C24(H24), C25(H25),
 C26(H26), C27(H27), C28(H28), C31(H31), C32(H32), C33(H33), C34(H34), C39(H39),
  C40(H40), C41(H41), C42(H42)
2.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C)
;
_olex2_submission_special_instructions 'No special instructions were received'