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_7706039
_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         'C41 H32 Mn2 N2 O5 P2'
_chemical_formula_sum            'C41 H32 Mn2 N2 O5 P2'
_chemical_formula_weight         804.50
_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             2020-06-11
_audit_creation_method
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Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
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_audit_update_record
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2020-06-14 deposited with the CCDC.	2020-12-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.0503(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.6738(3)
_cell_length_b                   9.62622(18)
_cell_length_c                   24.7524(5)
_cell_measurement_reflns_used    6021
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.7930
_cell_measurement_theta_min      3.7310
_cell_volume                     3734.63(13)
_computing_cell_refinement
;
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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_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)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2312
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -24.00   15.00   0.3900    6.5000
omega____ theta____ kappa____ phi______ frames
    -      -15.1755  -99.0000  -90.0000 100

  2 omega  -25.00   17.12   0.3900    6.5000
omega____ theta____ kappa____ phi______ frames
    -       18.0661  -99.0000   30.0000 108

  3 omega  -14.00   53.08   0.3900    6.5000
omega____ theta____ kappa____ phi______ frames
    -       18.0661  -99.0000 -180.0000 172

  4 omega  -10.00   29.00   0.3900    6.5000
omega____ theta____ kappa____ phi______ frames
    -       18.0661   19.0000  -30.0000 100

  5 omega   46.00   88.12   0.3900    6.5000
omega____ theta____ kappa____ phi______ frames
    -       18.0661   19.0000  -30.0000 108

  6 omega   -8.00   20.08   0.3900    6.5000
omega____ theta____ kappa____ phi______ frames
    -       18.0661  -77.0000   60.0000 72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0070961000
_diffrn_orient_matrix_UB_12      0.0638135000
_diffrn_orient_matrix_UB_13      -0.0135651000
_diffrn_orient_matrix_UB_21      -0.0332530000
_diffrn_orient_matrix_UB_22      0.0311201000
_diffrn_orient_matrix_UB_23      0.0151758000
_diffrn_orient_matrix_UB_31      0.0298580000
_diffrn_orient_matrix_UB_32      0.0195743000
_diffrn_orient_matrix_UB_33      0.0201946000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_unetI/netI     0.0518
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            18551
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.352
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.809
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94290
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_description       block
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.307
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.055
_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     473
_refine_ls_number_reflns         7605
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_gt           0.0428
_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^)+(0.0410P)^2^+0.5806P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0918
_refine_ls_wR_factor_ref         0.1011
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5673
_reflns_number_total             7605
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03934a2.cif
_cod_data_source_block           201710195
_cod_depositor_comments
'Adding full bibliography for 7706035--7706039.cif.'
_cod_original_cell_volume        3734.62(12)
_cod_database_code               7706039
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C40H40N2O2P2Mn1
_shelx_estimated_absorpt_t_max   0.895
_shelx_estimated_absorpt_t_min   0.868
_reflns_odcompleteness_completeness 99.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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:
 C10(H10), C11(H11)
2.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C25(H25), C26(H26),
 C27(H27), C28(H28), C30(H30), C31(H31), C32(H32), C33(H33), C37(H37), C38(H38),
  C39(H39), C40(H40), C41(H41)
2.c Idealised Me refined as rotating group:
 C22(H22a,H22b,H22c), C23(H23a,H23b,H23c), C34(H34a,H34b,H34c), C35(H35a,H35b,
 H35c)
;
_olex2_submission_special_instructions 'No special instructions were received'