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_7706037
_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         'C45 H38 Mn2 O7 P2'
_chemical_formula_sum            'C45 H38 Mn2 O7 P2'
_chemical_formula_weight         862.57
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-05-17
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Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
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_audit_update_record
;
2020-06-14 deposited with the CCDC.	2020-12-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.5276(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.67365(18)
_cell_length_b                   14.2261(3)
_cell_length_c                   26.7140(5)
_cell_measurement_reflns_used    5029
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.3730
_cell_measurement_theta_min      4.1400
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_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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)
;
_computing_data_reduction
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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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_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
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_diffrn_measured_fraction_theta_full 0.999
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_diffrn_measurement_details
;
  1 omega  -41.00   33.70   0.9000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000   57.0000  -60.0000 83

  2 omega  -56.00   -5.60   0.9000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000   77.0000 -120.0000 56

  3 omega  -35.00    3.70   0.9000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -19.0000  -90.0000 43

  4 omega  -29.00   11.50   0.9000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -37.0000 -150.0000 45

  5 omega   79.00  105.10   0.9000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  178.0000 -120.0000 29

  6 omega   70.00   96.10   0.9000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734   57.0000   90.0000 29

  7 omega   40.00   74.20   0.9000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -99.0000 -180.0000 38

  8 omega    9.00   99.00   0.9000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734   77.0000   30.0000 100

  9 omega   -3.00   30.30   0.9000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -99.0000 -180.0000 37

 10 omega   78.00  109.50   0.9000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  178.0000   30.0000 35

 11 omega   18.00   45.00   0.9000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -37.0000 -150.0000 30

 12 omega   39.00   65.10   0.9000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734   57.0000   90.0000 29

 13 omega   47.00   73.10   0.9000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -19.0000  -90.0000 29

 14 omega   31.00   57.10   0.9000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -99.0000  -90.0000 29

 15 omega   43.00   78.10   0.9000   27.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -30.0000 39

 16 omega   54.00   90.00   0.9000   27.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -90.0000 40

 17 omega   61.00  138.40   0.9000   27.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  178.0000   30.0000 86

 18 omega   97.00  167.20   0.9000   27.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000   30.0000 78

 19 omega   64.00  108.10   0.9000   27.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000 -180.0000 49

 20 omega   68.00  106.70   0.9000   27.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000   60.0000 43

 21 omega   47.00   80.30   0.9000   27.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000   60.0000 37

 22 omega  104.00  133.70   0.9000   27.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000   90.0000 33

 23 omega   38.80   91.00   0.9000   27.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000    0.0000 58

 24 omega   39.00  136.20   0.9000   27.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000  -60.0000 108
;
_diffrn_measurement_device       'four-circle diffractometer'
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_diffrn_orient_matrix_UB_11      -0.0291819000
_diffrn_orient_matrix_UB_12      0.1048257000
_diffrn_orient_matrix_UB_13      -0.0093309000
_diffrn_orient_matrix_UB_21      0.0351476000
_diffrn_orient_matrix_UB_22      0.0213342000
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_diffrn_orient_matrix_UB_31      0.1372169000
_diffrn_orient_matrix_UB_32      0.0168157000
_diffrn_orient_matrix_UB_33      -0.0124763000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_unetI/netI     0.0827
_diffrn_reflns_Laue_measured_fraction_full 0.999
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_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            16980
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.075
_diffrn_reflns_theta_max         67.075
_diffrn_reflns_theta_min         3.315
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.240
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77371
_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    1.415
_exptl_crystal_description       needle
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.499
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     511
_refine_ls_number_reflns         7210
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0891
_refine_ls_R_factor_gt           0.0536
_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^)+(0.0405P)^2^] where P=(Fo^2^+2Fc^2^)/3'
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_refine_ls_wR_factor_gt          0.1114
_refine_ls_wR_factor_ref         0.1232
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4783
_reflns_number_total             7210
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03934a2.cif
_cod_data_source_block           20170575
_cod_depositor_comments
'Adding full bibliography for 7706035--7706039.cif.'
_cod_original_cell_volume        4048.67(13)
_cod_database_code               7706037
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C38H70N2O2P2Cl2Mn1
_reflns_odcompleteness_completeness 99.88
_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
2.a Ternary CH refined with riding coordinates:
 C30(H30), C31(H31)
2.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C23(H23), C24(H24),
 C25(H25), C26(H26), C27(H27), C33(H33), C34(H34), C36(H36), C37(H37), C40(H40),
  C41(H41), C43(H43), C44(H44)
2.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C28(H28A,H28B,H28C), C29(H29A,H29B,
 H29C), C38(H38A,H38B,H38C), C45(H45A,H45B,H45C)
;
_olex2_submission_special_instructions 'No special instructions were received'