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_7033710
_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         'C19 H12 Cl O6 P W'
_chemical_formula_sum            'C19 H12 Cl O6 P W'
_chemical_formula_weight         586.56
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-09-25
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_audit_update_record
;
2014-09-25 deposited with the CCDC.
2015-01-19 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.502(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.4704(7)
_cell_length_b                   11.0754(5)
_cell_length_c                   14.5549(6)
_cell_measurement_reflns_used    2927
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      27.2630
_cell_measurement_theta_min      3.3350
_cell_volume                     2010.17(17)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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_area_resol_mean 16.2312
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -21.00    5.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.2104  -99.0000   90.0000 26

  2 omega  -25.00   20.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.2104  -99.0000  150.0000 45

  3 omega   58.00   96.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7885 -178.0000  120.0000 38

  4 omega   57.00   85.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7885  178.0000  -30.0000 28

  5 omega  -40.00   91.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7885    0.0000  -90.0000 131
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0448543000
_diffrn_orient_matrix_UB_12      -0.0371308000
_diffrn_orient_matrix_UB_13      0.0103319000
_diffrn_orient_matrix_UB_21      -0.0269930000
_diffrn_orient_matrix_UB_22      -0.0502654000
_diffrn_orient_matrix_UB_23      -0.0196672000
_diffrn_orient_matrix_UB_31      0.0223028000
_diffrn_orient_matrix_UB_32      0.0139860000
_diffrn_orient_matrix_UB_33      -0.0433596000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_unetI/netI     0.0470
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9588
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.27
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.991
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73364
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
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_density_diffrn    1.938
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.405
_refine_diff_density_min         -0.761
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         4099
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0332
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0222P)^2^+0.7800P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0616
_refine_ls_wR_factor_ref         0.0679
_reflns_number_gt                3299
_reflns_number_total             4099
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt03972f5.cif
_cod_data_source_block           201409188
_cod_depositor_comments
'Adding full bibliography for 7033709--7033710.cif.'
_cod_original_cell_volume        2010.16(17)
_cod_database_code               7033710
_chemical_oxdiff_formula         C11H20N1O1W1Cl1
_reflns_odcompleteness_completeness 99.70
_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:
 C18(H18)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C13(H13), C14(H14), C15(H15), C16(H16)
2.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C)
;
_olex2_submission_special_instructions 'No special instructions were received'