#------------------------------------------------------------------------------
#$Date: 2017-10-13 14:42:48 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201982 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/30/86/4308647.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_4308647
loop_
_publ_author_name
'Wolfgang Petz'
'Christian Kutschera'
'Maya Heitbaum'
'Gernot Frenking'
'Ralf Tonner'
'Bernhard Neumüller'
_publ_contact_author
;
        Gernot Frenking
        Fachbereich Chemie
        Universität Marburg
        Hans-Meerwein-Strasse
        35032 Marburg
        Germany
;
_publ_contact_author_email       frenking@chemie.uni-marburg.de
_publ_contact_author_fax         'int. 6421-28-25566'
_publ_contact_author_phone       'int. 6421-28-25563'
_publ_section_title
;
Experimental and Theoretical Studies of Carbodiphosphorane-CX2 Adducts
with Unusual Bonding Situations: Preparation, Crystal Structures, and
Bonding Analyses of S2CC(PPh3)2, O2CC(PPh3)2, and [(CO)4MS2CC(PPh3)2] (M =
Cr, Mo, W)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1263
_journal_page_last               1274
_journal_paper_doi               10.1021/ic048397l
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         '[O~2~CC(PPh~3~)~2~]'
_chemical_formula_sum            'C38 H30 O2 P2'
_chemical_formula_weight         580.56
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 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                 102.86(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.939(1)
_cell_length_b                   17.053(1)
_cell_length_c                   15.109(1)
_cell_measurement_reflns_used    15000
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      26.26
_cell_measurement_theta_min      2.12
_cell_volume                     2999.0(4)
_computing_cell_refinement       'IPDS II (Stoe)'
_computing_data_collection       'IPDS II (Stoe)'
_computing_data_reduction        'IPDS II (Stoe)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1996)'
_computing_publication_material
'SHELXL-97 (Sheldrick, 1997), PLATON-98 (Spek, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'IPDS II (Stoe)'
_diffrn_measurement_method       'IPDS II (Stoe)'
_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  0.0787
_diffrn_reflns_av_sigmaI/netI    0.0525
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21554
_diffrn_reflns_theta_full        26.28
_diffrn_reflns_theta_max         26.28
_diffrn_reflns_theta_min         2.12
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.179
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.44
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.186
_refine_diff_density_min         -0.216
_refine_diff_density_rms         0.040
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         5793
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0353
_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/[σ²(Fo²)+(0.0529P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0826
_refine_ls_wR_factor_ref         0.0873
_reflns_number_gt                4829
_reflns_number_total             5793
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048397lsi20041124_051054_2.cif
_cod_data_source_block           pe47
_cod_depositor_comments
;
The following automatic conversions were performed:
data name '_publ_contact_autor' replaced with '_publ_contact_author'
as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 4998 2017-03-02 13:24:31Z antanas 
;
_cod_database_code               4308647
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'
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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O -0.11921(14) 0.37155(10) 0.96193(11) 0.0492(4) Uani 1 1 d . . .
O2 O -0.01632(14) 0.37005(9) 0.85315(12) 0.0470(4) Uani 1 1 d . . .
C1 C -0.16913(18) 0.28310(12) 0.83986(15) 0.0377(5) Uani 1 1 d . . .
C2 C -0.09606(18) 0.34738(12) 0.88935(16) 0.0390(5) Uani 1 1 d . . .
P1 P -0.27191(4) 0.25152(3) 0.89550(3) 0.03471(13) Uani 1 1 d . . .
C3 C -0.20556(19) 0.21676(13) 1.00812(15) 0.0393(5) Uani 1 1 d . . .
C4 C -0.2482(2) 0.23292(15) 1.08446(16) 0.0474(6) Uani 1 1 d . . .
H41 H -0.3124 0.2668 1.0797 0.0631(15) Uiso 1 1 calc R . .
C5 C -0.1977(2) 0.19986(17) 1.16754(17) 0.0560(6) Uani 1 1 d . . .
H51 H -0.2273 0.2112 1.2195 0.0631(15) Uiso 1 1 calc R . .
C6 C -0.1055(2) 0.15106(16) 1.17496(18) 0.0546(6) Uani 1 1 d . . .
H61 H -0.0717 0.1281 1.2319 0.0631(15) Uiso 1 1 calc R . .
C7 C -0.0613(2) 0.13490(16) 1.10029(19) 0.0559(6) Uani 1 1 d . . .
H71 H 0.0030 0.1010 1.1059 0.0631(15) Uiso 1 1 calc R . .
C8 C -0.1104(2) 0.16784(15) 1.01714(17) 0.0475(5) Uani 1 1 d . . .
H81 H -0.0790 0.1570 0.9659 0.0631(15) Uiso 1 1 calc R . .
C9 C -0.35730(18) 0.17038(13) 0.84124(15) 0.0383(5) Uani 1 1 d . . .
C10 C -0.43139(19) 0.18208(13) 0.75647(16) 0.0414(5) Uani 1 1 d . . .
H101 H -0.4350 0.2320 0.7280 0.0631(15) Uiso 1 1 calc R . .
C11 C -0.4996(2) 0.12106(15) 0.71392(17) 0.0485(6) Uani 1 1 d . . .
H111 H -0.5485 0.1286 0.6557 0.0631(15) Uiso 1 1 calc R . .
C12 C -0.4958(2) 0.04887(15) 0.75689(18) 0.0508(6) Uani 1 1 d . . .
H121 H -0.5429 0.0071 0.7282 0.0631(15) Uiso 1 1 calc R . .
C13 C -0.4239(2) 0.03737(14) 0.84108(19) 0.0522(6) Uani 1 1 d . . .
H131 H -0.4222 -0.0121 0.8703 0.0631(15) Uiso 1 1 calc R . .
C14 C -0.3547(2) 0.09740(14) 0.88291(16) 0.0445(5) Uani 1 1 d . . .
H141 H -0.3049 0.0889 0.9406 0.0631(15) Uiso 1 1 calc R . .
C15 C -0.37988(19) 0.32501(13) 0.90518(15) 0.0399(5) Uani 1 1 d . . .
C16 C -0.4807(2) 0.30111(16) 0.92792(18) 0.0496(6) Uani 1 1 d . . .
H161 H -0.4925 0.2470 0.9379 0.0631(15) Uiso 1 1 calc R . .
C17 C -0.5648(2) 0.35498(18) 0.9363(2) 0.0589(7) Uani 1 1 d . . .
H171 H -0.6331 0.3379 0.9528 0.0631(15) Uiso 1 1 calc R . .
C18 C -0.5489(3) 0.43377(17) 0.9206(2) 0.0628(7) Uani 1 1 d . . .
H181 H -0.6057 0.4710 0.9271 0.0631(15) Uiso 1 1 calc R . .
C19 C -0.4501(2) 0.45801(15) 0.8954(2) 0.0575(7) Uani 1 1 d . . .
H191 H -0.4401 0.5119 0.8834 0.0631(15) Uiso 1 1 calc R . .
C20 C -0.3656(2) 0.40446(14) 0.88770(18) 0.0474(5) Uani 1 1 d . . .
H201 H -0.2978 0.4217 0.8705 0.0631(15) Uiso 1 1 calc R . .
P2 P -0.11950(4) 0.25137(3) 0.74800(3) 0.03411(13) Uani 1 1 d . . .
C21 C 0.02378(19) 0.20783(13) 0.77473(14) 0.0397(5) Uani 1 1 d . . .
C22 C 0.0601(2) 0.16187(15) 0.71034(17) 0.0464(5) Uani 1 1 d . . .
H221 H 0.0119 0.1559 0.6516 0.0631(15) Uiso 1 1 calc R . .
C23 C 0.1665(2) 0.12449(16) 0.7313(2) 0.0572(7) Uani 1 1 d . . .
H231 H 0.1912 0.0941 0.6865 0.0631(15) Uiso 1 1 calc R . .
C24 C 0.2360(2) 0.13157(17) 0.81725(19) 0.0565(6) Uani 1 1 d . . .
H241 H 0.3080 0.1053 0.8321 0.0631(15) Uiso 1 1 calc R . .
C25 C 0.2005(2) 0.17683(16) 0.88119(19) 0.0526(6) Uani 1 1 d . . .
H251 H 0.2488 0.1822 0.9400 0.0631(15) Uiso 1 1 calc R . .
C26 C 0.0955(2) 0.21469(14) 0.86106(16) 0.0433(5) Uani 1 1 d . . .
H261 H 0.0720 0.2455 0.9061 0.0631(15) Uiso 1 1 calc R . .
C27 C -0.20173(18) 0.17211(13) 0.68513(15) 0.0377(5) Uani 1 1 d . . .
C28 C -0.2704(2) 0.18359(14) 0.59873(16) 0.0445(5) Uani 1 1 d . . .
H281 H -0.2786 0.2346 0.5728 0.0631(15) Uiso 1 1 calc R . .
C29 C -0.3269(2) 0.12035(16) 0.55043(18) 0.0536(6) Uani 1 1 d . . .
H291 H -0.3736 0.1280 0.4914 0.0631(15) Uiso 1 1 calc R . .
C30 C -0.3150(2) 0.04690(16) 0.58828(19) 0.0563(7) Uani 1 1 d . . .
H301 H -0.3534 0.0038 0.5549 0.0631(15) Uiso 1 1 calc R . .
C31 C -0.2479(2) 0.03484(14) 0.6744(2) 0.0527(6) Uani 1 1 d . . .
H311 H -0.2413 -0.0161 0.7004 0.0631(15) Uiso 1 1 calc R . .
C32 C -0.1904(2) 0.09722(13) 0.72230(17) 0.0437(5) Uani 1 1 d . . .
H321 H -0.1429 0.0889 0.7809 0.0631(15) Uiso 1 1 calc R . .
C33 C -0.12375(18) 0.33037(13) 0.66708(15) 0.0394(5) Uani 1 1 d . . .
C34 C -0.2146(2) 0.38269(13) 0.65384(16) 0.0444(5) Uani 1 1 d . . .
H341 H -0.2725 0.3772 0.6876 0.0631(15) Uiso 1 1 calc R . .
C35 C -0.2215(3) 0.44359(15) 0.59099(18) 0.0550(6) Uani 1 1 d . . .
H351 H -0.2841 0.4792 0.5821 0.0631(15) Uiso 1 1 calc R . .
C36 C -0.1379(3) 0.45218(15) 0.54194(17) 0.0569(7) Uani 1 1 d . . .
H361 H -0.1420 0.4942 0.5000 0.0631(15) Uiso 1 1 calc R . .
C37 C -0.0488(2) 0.39978(15) 0.55392(17) 0.0537(6) Uani 1 1 d . . .
H371 H 0.0079 0.4050 0.5191 0.0631(15) Uiso 1 1 calc R . .
C38 C -0.0403(2) 0.33894(15) 0.61652(16) 0.0462(5) Uani 1 1 d . . .
H381 H 0.0224 0.3033 0.6247 0.0631(15) Uiso 1 1 calc R . .
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'
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
C2 C1 P2 111.62(15) . . ?
C2 C1 P1 112.68(15) . . ?
P2 C1 P1 135.20(13) . . ?
O1 C2 O2 127.7(2) . . ?
O1 C2 C1 117.35(19) . . ?
O2 C2 C1 114.92(19) . . ?
C1 P1 C9 114.22(10) . . ?
C1 P1 C3 110.57(10) . . ?
C9 P1 C3 105.13(10) . . ?
C1 P1 C15 114.64(10) . . ?
C9 P1 C15 103.01(10) . . ?
C3 P1 C15 108.57(10) . . ?
C4 C3 C8 118.7(2) . . ?
C4 C3 P1 123.48(18) . . ?
C8 C3 P1 117.75(17) . . ?
C5 C4 C3 120.4(2) . . ?
C6 C5 C4 120.2(2) . . ?
C5 C6 C7 120.3(2) . . ?
C6 C7 C8 120.1(3) . . ?
C7 C8 C3 120.3(2) . . ?
C14 C9 C10 119.2(2) . . ?
C14 C9 P1 121.79(18) . . ?
C10 C9 P1 119.00(17) . . ?
C11 C10 C9 120.2(2) . . ?
C10 C11 C12 119.6(2) . . ?
C13 C12 C11 120.4(2) . . ?
C14 C13 C12 120.2(2) . . ?
C13 C14 C9 120.4(2) . . ?
C16 C15 C20 118.8(2) . . ?
C16 C15 P1 119.07(18) . . ?
C20 C15 P1 122.11(17) . . ?
C15 C16 C17 121.0(2) . . ?
C18 C17 C16 119.8(3) . . ?
C19 C18 C17 119.8(2) . . ?
C18 C19 C20 120.6(3) . . ?
C19 C20 C15 120.0(2) . . ?
C1 P2 C27 114.57(10) . . ?
C1 P2 C33 110.41(10) . . ?
C27 P2 C33 105.70(10) . . ?
C1 P2 C21 115.16(10) . . ?
C27 P2 C21 100.63(10) . . ?
C33 P2 C21 109.62(10) . . ?
C22 C21 C26 118.6(2) . . ?
C22 C21 P2 119.79(18) . . ?
C26 C21 P2 121.46(16) . . ?
C21 C22 C23 120.6(2) . . ?
C24 C23 C22 120.0(2) . . ?
C25 C24 C23 119.6(2) . . ?
C24 C25 C26 120.9(3) . . ?
C25 C26 C21 120.2(2) . . ?
C32 C27 C28 119.5(2) . . ?
C32 C27 P2 118.78(18) . . ?
C28 C27 P2 121.62(18) . . ?
C29 C28 C27 119.9(2) . . ?
C30 C29 C28 119.8(3) . . ?
C29 C30 C31 120.8(2) . . ?
C32 C31 C30 119.7(2) . . ?
C31 C32 C27 120.3(2) . . ?
C34 C33 C38 119.1(2) . . ?
C34 C33 P2 118.69(16) . . ?
C38 C33 P2 122.17(18) . . ?
C33 C34 C35 120.2(2) . . ?
C36 C35 C34 120.3(2) . . ?
C37 C36 C35 119.6(2) . . ?
C36 C37 C38 120.8(2) . . ?
C33 C38 C37 119.9(2) . . ?
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
O1 C2 1.258(3) . ?
O2 C2 1.260(3) . ?
C1 C2 1.494(3) . ?
C1 P2 1.714(2) . ?
C1 P1 1.721(2) . ?
P1 C9 1.804(2) . ?
P1 C3 1.809(2) . ?
P1 C15 1.827(2) . ?
C3 C4 1.388(3) . ?
C3 C8 1.391(3) . ?
C4 C5 1.386(4) . ?
C5 C6 1.364(4) . ?
C6 C7 1.375(4) . ?
C7 C8 1.382(4) . ?
C9 C14 1.392(3) . ?
C9 C10 1.399(3) . ?
C10 C11 1.388(3) . ?
C11 C12 1.388(4) . ?
C12 C13 1.381(4) . ?
C13 C14 1.378(3) . ?
C15 C16 1.385(3) . ?
C15 C20 1.398(3) . ?
C16 C17 1.387(4) . ?
C17 C18 1.385(4) . ?
C18 C19 1.380(4) . ?
C19 C20 1.386(3) . ?
P2 C27 1.811(2) . ?
P2 C33 1.812(2) . ?
P2 C21 1.826(2) . ?
C21 C22 1.392(3) . ?
C21 C26 1.397(3) . ?
C22 C23 1.393(4) . ?
C23 C24 1.382(4) . ?
C24 C25 1.375(4) . ?
C25 C26 1.383(3) . ?
C27 C32 1.390(3) . ?
C27 C28 1.392(3) . ?
C28 C29 1.390(3) . ?
C29 C30 1.371(4) . ?
C30 C31 1.383(4) . ?
C31 C32 1.380(4) . ?
C33 C34 1.384(3) . ?
C33 C38 1.392(3) . ?
C34 C35 1.397(3) . ?
C35 C36 1.376(4) . ?
C36 C37 1.370(4) . ?
C37 C38 1.392(4) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30660853
