6-Methoxy-5-phosphaphenanthrene: a molecule with an unreactive P[double bond, length as m-dash]C double bond.
Wang, Lili; Wang, Zhihua; Wang, Qiuyan; Duan, Zheng; Mathey, François; Dalton transactions (Cambridge, England : 2003) 44 (2015) 3717–3719; doi:10.1039/c4dt03972f

data_7033709
_publ_section_title
;
 6-Methoxy-5-phosphaphenanthrene: a molecule with an unreactive P[double
 bond, length as m-dash]C double bond.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3717
_journal_page_last               3719
_journal_paper_doi               10.1039/c4dt03972f
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         '2(C19 H11 O5.95 P W)'
_chemical_formula_sum            'C38 H22 O12 P2 W2'
_chemical_formula_weight         1100.20
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-09-19
_audit_creation_method
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_audit_update_record
;
2014-09-22 deposited with the CCDC.
2015-01-19 downloaded from the CCDC.
;
_cell_angle_alpha                63.056(6)
_cell_angle_beta                 74.408(5)
_cell_angle_gamma                84.555(5)
_cell_formula_units_Z            2
_cell_length_a                   11.5815(7)
_cell_length_b                   13.2137(7)
_cell_length_c                   14.4201(10)
_cell_measurement_reflns_used    3910
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      25.3030
_cell_measurement_theta_min      3.2620
_cell_volume                     1893.9(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      291.15
_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 0.997
_diffrn_measurement_details
;
  1 omega  -20.00   25.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.2104  -99.0000  -60.0000 45

  2 omega  -48.00   46.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7885  -37.0000  -30.0000 94

  3 omega  -10.00   74.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7885   77.0000 -120.0000 84

  4 omega   48.00   85.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7885  178.0000    0.0000 37

  5 omega  -24.00   87.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7885   19.0000 -180.0000 111

  6 omega   21.00   62.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7885  -99.0000  120.0000 41

  7 omega  -53.00  -16.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7885    0.0000   60.0000 37
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0216523000
_diffrn_orient_matrix_UB_12      0.0255962000
_diffrn_orient_matrix_UB_13      0.0350398000
_diffrn_orient_matrix_UB_21      -0.0464838000
_diffrn_orient_matrix_UB_22      0.0248358000
_diffrn_orient_matrix_UB_23      -0.0261426000
_diffrn_orient_matrix_UB_31      -0.0376386000
_diffrn_orient_matrix_UB_32      -0.0485569000
_diffrn_orient_matrix_UB_33      0.0366402000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_unetI/netI     0.0673
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15675
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.13
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.216
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36853
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.929
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         5.899
_refine_diff_density_min         -1.676
_refine_diff_density_rms         0.233
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     490
_refine_ls_number_reflns         7707
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1055
_refine_ls_R_factor_gt           0.0741
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1251P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1825
_refine_ls_wR_factor_ref         0.2109
_reflns_number_gt                5265
_reflns_number_total             7707
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt03972f5.cif
_cod_data_source_block           201409183
_cod_depositor_comments
'Adding full bibliography for 7033709--7033710.cif.'
_cod_original_cell_volume        1893.91(19)
_cod_database_code               7033709
_chemical_oxdiff_formula         C20H20O4P1W1
_reflns_odcompleteness_completeness 99.84
_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 Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C13(H13), C14(H14), C15(H15), C16(H16),
 C6'(H6'), C7'(H7'), C8'(H8'), C9'(H9'), C13'(H13'), C14'(H14'), C15'(H15'),
 C16'(H16')
2.b Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C19'(H19D,H19E,H19F)
;
_olex2_submission_special_instructions 'No special instructions were received'