A new route to a 2-phosphanaphthalene.
Mao, Yanli; Lim, Kelvin Meng Hui; Ganguly, Rakesh; Mathey, Francois; Organic letters 14 (2012) 4974–4975; doi:10.1021/ol302278p

data_1516057
_publ_section_title
;
 A new route to a 2-phosphanaphthalene.
;
_journal_issue                   18
_journal_name_full               'Organic letters'
_journal_page_first              4974
_journal_page_last               4975
_journal_paper_doi               10.1021/ol302278p
_journal_volume                  14
_journal_year                    2012
_chemical_formula_moiety         'C26 H15 Mo O5 P'
_chemical_formula_sum            'C26 H15 Mo O5 P'
_chemical_formula_weight         534.29
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.831(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.039(5)
_cell_length_b                   6.2992(13)
_cell_length_c                   21.025(6)
_cell_measurement_reflns_used    1807
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      21.83
_cell_measurement_theta_min      2.93
_cell_volume                     2235.6(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1104
_diffrn_reflns_av_sigmaI/netI    0.1889
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            30153
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         33.19
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    0.694
_exptl_absorpt_correction_T_max  0.9728
_exptl_absorpt_correction_T_min  0.7686
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.186
_refine_diff_density_min         -1.952
_refine_diff_density_rms         0.246
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.07(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         14325
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.970
_refine_ls_R_factor_all          0.1402
_refine_ls_R_factor_gt           0.0704
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0905P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1455
_refine_ls_wR_factor_ref         0.2063
_reflns_number_gt                8514
_reflns_number_total             14325
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            mat141.cif
_cod_data_source_block           mat141
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        2235.6(11)
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               1516057