#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:37:02 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179338 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/35/4323513.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4323513
loop_
_publ_author_name
'Klaus Eichele'
'Roderick E. Wasylishen'
'Kalyani Maitra'
'John H. Nelson'
'James F. Britten'
_publ_section_title
;
 Single-Crystal 31P NMR and X-ray Diffraction Study of a Molybdenum
 Phosphine Complex: (5-Methyldibenzophosphole)pentacarbonylmolybdenum(0)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3539
_journal_page_last               3544
_journal_paper_doi               10.1021/ic970260q
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C18 H11 Mo O5 P'
_chemical_formula_weight         434.18
_chemical_name_systematic        ?
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 122.135(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   31.113(2)
_cell_length_b                   7.7917(5)
_cell_length_c                   17.9522(12)
_cell_measurement_reflns_used    27
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      12.49
_cell_measurement_theta_min      5.11
_cell_volume                     3685.3(4)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-93 (Sheldrick, 1993)'
_diffrn_ambient_temperature      298(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       'ω 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  0.0161
_diffrn_reflns_av_sigmaI/netI    0.0185
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            3022
_diffrn_reflns_theta_max         22.49
_diffrn_reflns_theta_min         2.27
_diffrn_standards_decay_%        0.69
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.822
_exptl_absorpt_correction_T_max  0.6118
_exptl_absorpt_correction_T_min  0.5626
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            pale_yellow
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_description       rhomb
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          .40
_exptl_crystal_size_mid          .55
_exptl_crystal_size_min          .68
_refine_diff_density_max         0.279
_refine_diff_density_min         -0.223
_refine_diff_density_rms         0.046
_refine_ls_extinction_coef       0.00099(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.104
_refine_ls_goodness_of_fit_obs   1.131
_refine_ls_hydrogen_treatment    'riding model with fixed U'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         2407
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_restrained_S_obs      1.131
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_obs          0.0245
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0281P)²+4.3206P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0609
_refine_ls_wR_factor_obs         0.0584
_reflns_number_observed          2137
_reflns_number_total             2407
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic970260q.cif
_cod_data_source_block           vjc129
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0281P)^2^+4.3206P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0281P)^2^+4.3206P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3685.2(4)
_cod_database_code               4323513
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Mo1 Mo 0.075680(10) 0.92919(4) 0.46467(2) 0.04264(13) Uani 1 d . .
P1 P 0.12762(3) 0.66256(11) 0.51837(5) 0.0428(2) Uani 1 d . .
O1 O -0.02099(11) 0.6892(4) 0.3956(2) 0.0911(9) Uani 1 d . .
O2 O 0.09193(11) 0.9553(4) 0.6538(2) 0.0892(9) Uani 1 d . .
O3 O 0.00728(10) 1.2593(4) 0.3960(2) 0.0938(9) Uani 1 d . .
O4 O 0.17725(10) 1.1449(4) 0.5450(2) 0.0815(8) Uani 1 d . .
O5 O 0.06830(14) 0.9015(5) 0.2824(2) 0.1152(12) Uani 1 d . .
C1 C 0.01293(13) 0.7760(5) 0.4196(2) 0.0573(9) Uani 1 d . .
C2 C 0.08454(13) 0.9479(5) 0.5850(3) 0.0574(9) Uani 1 d . .
C3 C 0.03210(13) 1.1397(5) 0.4212(3) 0.0632(10) Uani 1 d . .
C4 C 0.14055(14) 1.0697(5) 0.5142(2) 0.0541(8) Uani 1 d . .
C5 C 0.07084(14) 0.9102(5) 0.3473(2) 0.0658(10) Uani 1 d . .
C6 C 0.10808(14) 0.5084(5) 0.5719(2) 0.0613(9) Uani 1 d . .
H6A H 0.0732(3) 0.4775(24) 0.5321(6) 0.092 Uiso 1 calc R .
H6B H 0.1119(9) 0.5594(12) 0.6238(9) 0.092 Uiso 1 calc R .
H6C H 0.1289(6) 0.4076(13) 0.5879(14) 0.092 Uiso 1 calc R .
C7 C 0.19571(12) 0.6801(4) 0.5931(2) 0.0535(9) Uani 1 d . .
C8 C 0.22145(15) 0.7649(5) 0.6730(2) 0.0777(12) Uani 1 d . .
H8A H 0.20388(15) 0.8202(5) 0.6948(2) 0.093 Uiso 1 calc R .
C9 C 0.2739(2) 0.7656(7) 0.7197(3) 0.109(2) Uani 1 d . .
H9A H 0.2919(2) 0.8211(7) 0.7738(3) 0.131 Uiso 1 calc R .
C10 C 0.2997(2) 0.6846(9) 0.6867(4) 0.122(2) Uani 1 d . .
H10A H 0.3350(2) 0.6858(9) 0.7191(4) 0.147 Uiso 1 calc R .
C11 C 0.2743(2) 0.6019(6) 0.6067(4) 0.097(2) Uani 1 d . .
H11A H 0.2923(2) 0.5494(6) 0.5850(4) 0.117 Uiso 1 calc R .
C12 C 0.22120(13) 0.5973(5) 0.5584(3) 0.0630(10) Uani 1 d . .
C13 C 0.18762(14) 0.5149(5) 0.4733(2) 0.0581(9) Uani 1 d . .
C14 C 0.2009(2) 0.4214(6) 0.4219(4) 0.0881(14) Uani 1 d . .
H14A H 0.2348(2) 0.4064(6) 0.4405(4) 0.106 Uiso 1 calc R .
C15 C 0.1629(3) 0.3518(6) 0.3433(4) 0.102(2) Uani 1 d . .
H15A H 0.1717(3) 0.2890(6) 0.3093(4) 0.122 Uiso 1 calc R .
C16 C 0.1132(2) 0.3727(6) 0.3143(3) 0.0930(15) Uani 1 d . .
H16A H 0.0885(2) 0.3242(6) 0.2611(3) 0.112 Uiso 1 calc R .
C17 C 0.0994(2) 0.4653(5) 0.3633(2) 0.0689(11) Uani 1 d . .
H17A H 0.0653(2) 0.4810(5) 0.3432(2) 0.083 Uiso 1 calc R .
C18 C 0.13647(13) 0.5352(4) 0.4429(2) 0.0493(8) Uani 1 d . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C3 Mo1 C2 92.09(15) . . ?
C3 Mo1 C5 89.6(2) . . ?
C2 Mo1 C5 177.00(14) . . ?
C3 Mo1 C4 92.18(14) . . ?
C2 Mo1 C4 87.42(14) . . ?
C5 Mo1 C4 90.07(14) . . ?
C3 Mo1 C1 91.01(14) . . ?
C2 Mo1 C1 91.35(13) . . ?
C5 Mo1 C1 91.06(14) . . ?
C4 Mo1 C1 176.62(13) . . ?
C3 Mo1 P1 178.23(10) . . ?
C2 Mo1 P1 87.44(10) . . ?
C5 Mo1 P1 90.90(11) . . ?
C4 Mo1 P1 89.50(9) . . ?
C1 Mo1 P1 87.30(10) . . ?
C7 P1 C18 90.7(2) . . ?
C7 P1 C6 104.2(2) . . ?
C18 P1 C6 104.9(2) . . ?
C7 P1 Mo1 119.09(11) . . ?
C18 P1 Mo1 119.47(11) . . ?
C6 P1 Mo1 114.95(12) . . ?
O1 C1 Mo1 178.7(3) . . ?
O2 C2 Mo1 176.5(3) . . ?
O3 C3 Mo1 179.7(4) . . ?
O4 C4 Mo1 177.2(3) . . ?
O5 C5 Mo1 179.3(4) . . ?
C8 C7 C12 121.9(3) . . ?
C8 C7 P1 127.4(3) . . ?
C12 C7 P1 110.6(3) . . ?
C9 C8 C7 118.4(5) . . ?
C10 C9 C8 120.5(5) . . ?
C11 C10 C9 121.4(5) . . ?
C10 C11 C12 119.5(5) . . ?
C7 C12 C11 118.3(4) . . ?
C7 C12 C13 114.1(3) . . ?
C11 C12 C13 127.7(4) . . ?
C18 C13 C14 118.5(4) . . ?
C18 C13 C12 113.2(3) . . ?
C14 C13 C12 128.3(4) . . ?
C15 C14 C13 119.1(4) . . ?
C16 C15 C14 121.8(4) . . ?
C15 C16 C17 120.0(5) . . ?
C16 C17 C18 119.7(4) . . ?
C17 C18 C13 120.9(3) . . ?
C17 C18 P1 127.7(3) . . ?
C13 C18 P1 111.4(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 C3 2.003(4) . ?
Mo1 C2 2.032(4) . ?
Mo1 C5 2.035(4) . ?
Mo1 C4 2.038(4) . ?
Mo1 C1 2.052(4) . ?
Mo1 P1 2.4899(9) . ?
P1 C7 1.812(3) . ?
P1 C18 1.815(3) . ?
P1 C6 1.832(3) . ?
O1 C1 1.128(4) . ?
O2 C2 1.132(4) . ?
O3 C3 1.139(4) . ?
O4 C4 1.132(4) . ?
O5 C5 1.128(4) . ?
C7 C8 1.383(5) . ?
C7 C12 1.400(5) . ?
C8 C9 1.383(6) . ?
C9 C10 1.378(8) . ?
C10 C11 1.375(8) . ?
C11 C12 1.400(5) . ?
C12 C13 1.462(5) . ?
C13 C18 1.389(5) . ?
C13 C14 1.399(5) . ?
C14 C15 1.382(7) . ?
C15 C16 1.353(7) . ?
C16 C17 1.373(5) . ?
C17 C18 1.383(5) . ?
