#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:46:34 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179935 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/30/7023030.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_7023030
loop_
_publ_author_name
'Albrecht, Carolin'
'Schneider, Eva'
'Engeser, Marianne'
'Schnakenburg, Gregor'
'Espinosa, Arturo'
'Streubel, Rainer'
_publ_section_title
;
 Synthesis and DFT calculations of spirooxaphosphirane complexes.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8897
_journal_page_last               8906
_journal_paper_doi               10.1039/c3dt50556a
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C19 H21 Cr O6 P'
_chemical_formula_sum            'C19 H21 Cr O6 P'
_chemical_formula_weight         428.33
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 97.174(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.5967(5)
_cell_length_b                   13.9514(6)
_cell_length_c                   12.2801(5)
_cell_measurement_reflns_used    4557
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      29.13
_cell_measurement_theta_min      1.00
_cell_volume                     1971.25(14)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_sigmaI/netI    0.0393
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15154
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.22
_exptl_absorpt_coefficient_mu    0.693
_exptl_absorpt_correction_T_max  0.9728
_exptl_absorpt_correction_T_min  0.8912
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.807
_refine_diff_density_min         -0.395
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         4679
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0336
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0510P)²+0.6537P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0903
_refine_ls_wR_factor_ref         0.0953
_reflns_number_gt                3872
_reflns_number_total             4679
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt50556a.txt
_cod_data_source_block           Greg1843
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-Scan' changed to
'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7023030
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
C1 C 0.25991(15) 1.01634(12) 0.93135(14) 0.0225(4) Uani 1 1 d .
C2 C 0.32101(16) 1.10414(13) 0.98645(15) 0.0255(4) Uani 1 1 d .
H2A H 0.3125 1.1629 0.9410 0.031 Uiso 1 1 calc R
H2B H 0.4033 1.0929 1.0158 0.031 Uiso 1 1 calc R
C3 C 0.23604(19) 1.09855(17) 1.07439(19) 0.0407(5) Uani 1 1 d .
H3A H 0.2728 1.0752 1.1466 0.049 Uiso 1 1 calc R
H3B H 0.1928 1.1588 1.0824 0.049 Uiso 1 1 calc R
C4 C 0.16456(17) 1.02178(14) 1.00649(15) 0.0283(4) Uani 1 1 d .
H4A H 0.1545 0.9618 1.0474 0.034 Uiso 1 1 calc R
H4B H 0.0891 1.0453 0.9695 0.034 Uiso 1 1 calc R
C5 C 0.37531(14) 0.99293(12) 0.72602(13) 0.0186(3) Uani 1 1 d .
C6 C 0.41833(14) 0.90147(12) 0.67799(14) 0.0198(3) Uani 1 1 d .
C7 C 0.39064(15) 0.90329(12) 0.56813(14) 0.0221(4) Uani 1 1 d .
C8 C 0.33117(15) 0.99413(13) 0.53596(14) 0.0223(4) Uani 1 1 d .
C9 C 0.31915(15) 1.04599(12) 0.62638(14) 0.0207(3) Uani 1 1 d .
C10 C 0.47134(15) 1.04961(12) 0.79398(14) 0.0234(4) Uani 1 1 d .
H10A H 0.5356 1.0603 0.7505 0.028 Uiso 1 1 calc R
H10B H 0.4996 1.0134 0.8604 0.028 Uiso 1 1 calc R
H10C H 0.4405 1.1115 0.8147 0.028 Uiso 1 1 calc R
C11 C 0.48548(16) 0.82679(13) 0.74638(15) 0.0255(4) Uani 1 1 d .
H11A H 0.4530 0.8193 0.8158 0.031 Uiso 1 1 calc R
H11B H 0.5670 0.8465 0.7614 0.031 Uiso 1 1 calc R
H11C H 0.4805 0.7657 0.7068 0.031 Uiso 1 1 calc R
C12 C 0.41536(19) 0.82765(15) 0.48781(17) 0.0334(4) Uani 1 1 d .
H12A H 0.4475 0.7709 0.5276 0.040 Uiso 1 1 calc R
H12B H 0.4716 0.8522 0.4414 0.040 Uiso 1 1 calc R
H12C H 0.3431 0.8103 0.4418 0.040 Uiso 1 1 calc R
C13 C 0.29418(17) 1.02170(15) 0.41904(15) 0.0310(4) Uani 1 1 d .
H13A H 0.2545 0.9675 0.3799 0.037 Uiso 1 1 calc R
H13B H 0.3627 1.0391 0.3841 0.037 Uiso 1 1 calc R
H13C H 0.2411 1.0765 0.4166 0.037 Uiso 1 1 calc R
C14 C 0.26379(18) 1.14227(13) 0.63342(17) 0.0305(4) Uani 1 1 d .
H14A H 0.3233 1.1895 0.6600 0.037 Uiso 1 1 calc R
H14C H 0.2052 1.1391 0.6843 0.037 Uiso 1 1 calc R
H14B H 0.2266 1.1613 0.5606 0.037 Uiso 1 1 calc R
C17 C 0.00548(16) 0.97672(13) 0.75202(14) 0.0232(3) Uani 1 1 d U
C16 C 0.07775(16) 0.82385(13) 0.87586(15) 0.0246(4) Uani 1 1 d U
C18 C 0.09392(15) 0.89993(12) 0.58129(14) 0.0226(3) Uani 1 1 d U
C19 C 0.19111(16) 0.75780(13) 0.71010(15) 0.0242(4) Uani 1 1 d U
C15 C -0.03852(17) 0.79339(13) 0.68449(15) 0.0264(4) Uani 1 1 d U
Cr Cr 0.09419(2) 0.865110(18) 0.73184(2) 0.01832(9) Uani 1 1 d U
O1 O 0.32331(11) 0.92400(9) 0.92909(10) 0.0243(3) Uani 1 1 d .
O2 O -0.11998(13) 0.74935(11) 0.65552(13) 0.0407(4) Uani 1 1 d .
O3 O 0.06257(14) 0.79761(10) 0.96109(11) 0.0372(3) Uani 1 1 d .
O4 O -0.04642(13) 1.04473(10) 0.76437(11) 0.0344(3) Uani 1 1 d U
O5 O 0.08153(12) 0.91579(10) 0.48974(10) 0.0322(3) Uani 1 1 d U
O6 O 0.24660(12) 0.69259(10) 0.69635(13) 0.0353(3) Uani 1 1 d U
P P 0.25635(4) 0.95296(3) 0.80454(3) 0.01737(11) Uani 1 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'
Cr Cr 0.3209 0.6236 '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
O1 C1 C4 116.85(14)
O1 C1 C2 119.98(14)
C4 C1 C2 91.33(13)
O1 C1 P 60.80(8)
C4 C1 P 127.68(13)
C2 C1 P 137.79(13)
C1 C2 C3 88.18(14)
C1 C2 H2A 114.0
C3 C2 H2A 114.0
C1 C2 H2B 114.0
C3 C2 H2B 114.0
H2A C2 H2B 111.2
C4 C3 C2 90.22(14)
C4 C3 H3A 113.6
C2 C3 H3A 113.6
C4 C3 H3B 113.6
C2 C3 H3B 113.6
H3A C3 H3B 110.9
C1 C4 C3 88.87(14)
C1 C4 H4A 113.8
C3 C4 H4A 113.8
C1 C4 H4B 113.8
C3 C4 H4B 113.8
H4A C4 H4B 111.1
C9 C5 C6 103.15(13)
C9 C5 C10 113.66(14)
C6 C5 C10 113.30(14)
C9 C5 P 107.11(11)
C6 C5 P 104.48(11)
C10 C5 P 114.12(11)
C7 C6 C11 128.18(16)
C7 C6 C5 108.95(15)
C11 C6 C5 122.80(15)
C6 C7 C8 109.25(15)
C6 C7 C12 127.25(17)
C8 C7 C12 123.49(16)
C9 C8 C7 109.53(15)
C9 C8 C13 127.31(17)
C7 C8 C13 123.15(16)
C8 C9 C14 128.26(16)
C8 C9 C5 109.07(14)
C14 C9 C5 122.64(15)
C5 C10 H10A 109.5
C5 C10 H10B 109.5
H10A C10 H10B 109.5
C5 C10 H10C 109.5
H10A C10 H10C 109.5
H10B C10 H10C 109.5
C6 C11 H11A 109.5
C6 C11 H11B 109.5
H11A C11 H11B 109.5
C6 C11 H11C 109.5
H11A C11 H11C 109.5
H11B C11 H11C 109.5
C7 C12 H12A 109.5
C7 C12 H12B 109.5
H12A C12 H12B 109.5
C7 C12 H12C 109.5
H12A C12 H12C 109.5
H12B C12 H12C 109.5
C8 C13 H13A 109.5
C8 C13 H13B 109.5
H13A C13 H13B 109.5
C8 C13 H13C 109.5
H13A C13 H13C 109.5
H13B C13 H13C 109.5
C9 C14 H14A 109.5
C9 C14 H14C 109.5
H14A C14 H14C 109.5
C9 C14 H14B 109.5
H14A C14 H14B 109.5
H14C C14 H14B 109.5
O4 C17 Cr 178.96(16)
O3 C16 Cr 176.75(17)
O5 C18 Cr 172.11(16)
O6 C19 Cr 178.38(16)
O2 C15 Cr 179.9(2)
C15 Cr C16 87.29(8)
C15 Cr C17 92.36(8)
C16 Cr C17 90.46(8)
C15 Cr C19 90.74(8)
C16 Cr C19 91.26(8)
C17 Cr C19 176.52(8)
C15 Cr C18 86.17(8)
C16 Cr C18 173.41(8)
C17 Cr C18 88.99(7)
C19 Cr C18 89.65(8)
C15 Cr P 175.62(6)
C16 Cr P 88.42(6)
C17 Cr P 86.74(6)
C19 Cr P 90.28(5)
C18 Cr P 98.10(5)
C1 O1 P 68.53(8)
O1 P C1 50.67(7)
O1 P C5 104.82(7)
C1 P C5 111.38(8)
O1 P Cr 118.90(5)
C1 P Cr 121.64(6)
C5 P Cr 125.01(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 O1 1.485(2)
C1 C4 1.528(2)
C1 C2 1.530(2)
C1 P 1.7868(17)
C2 C3 1.552(3)
C2 H2A 0.9900
C2 H2B 0.9900
C3 C4 1.535(3)
C3 H3A 0.9900
C3 H3B 0.9900
C4 H4A 0.9900
C4 H4B 0.9900
C5 C9 1.507(2)
C5 C6 1.516(2)
C5 C10 1.526(2)
C5 P 1.8644(16)
C6 C7 1.347(2)
C6 C11 1.495(2)
C7 C8 1.473(2)
C7 C12 1.496(2)
C8 C9 1.347(2)
C8 C13 1.497(2)
C9 C14 1.496(2)
C10 H10A 0.9800
C10 H10B 0.9800
C10 H10C 0.9800
C11 H11A 0.9800
C11 H11B 0.9800
C11 H11C 0.9800
C12 H12A 0.9800
C12 H12B 0.9800
C12 H12C 0.9800
C13 H13A 0.9800
C13 H13B 0.9800
C13 H13C 0.9800
C14 H14A 0.9800
C14 H14C 0.9800
C14 H14B 0.9800
C17 O4 1.144(2)
C17 Cr 1.8994(19)
C16 O3 1.143(2)
C16 Cr 1.8920(18)
C18 O5 1.137(2)
C18 Cr 1.9112(18)
C19 O6 1.139(2)
C19 Cr 1.9107(19)
C15 O2 1.146(2)
C15 Cr 1.8666(19)
Cr P 2.3273(5)
O1 P 1.6760(13)
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
O1 C1 C2 C3 -113.41(17)
C4 C1 C2 C3 8.92(16)
P C1 C2 C3 168.26(19)
C1 C2 C3 C4 -8.88(16)
O1 C1 C4 C3 115.87(17)
C2 C1 C4 C3 -9.02(16)
P C1 C4 C3 -171.59(16)
C2 C3 C4 C1 8.89(16)
C9 C5 C6 C7 0.13(18)
C10 C5 C6 C7 -123.20(16)
P C5 C6 C7 112.00(13)
C9 C5 C6 C11 177.32(15)
C10 C5 C6 C11 54.0(2)
P C5 C6 C11 -70.81(18)
C11 C6 C7 C8 -175.89(16)
C5 C6 C7 C8 1.11(19)
C11 C6 C7 C12 3.5(3)
C5 C6 C7 C12 -179.49(17)
C6 C7 C8 C9 -2.1(2)
C12 C7 C8 C9 178.47(17)
C6 C7 C8 C13 176.63(16)
C12 C7 C8 C13 -2.8(3)
C7 C8 C9 C14 -179.68(17)
C13 C8 C9 C14 1.7(3)
C7 C8 C9 C5 2.14(19)
C13 C8 C9 C5 -176.52(16)
C6 C5 C9 C8 -1.43(18)
C10 C5 C9 C8 121.65(16)
P C5 C9 C8 -111.35(14)
C6 C5 C9 C14 -179.73(16)
C10 C5 C9 C14 -56.6(2)
P C5 C9 C14 70.35(18)
O2 C15 Cr C16 6(100)
O2 C15 Cr C17 -84(100)
O2 C15 Cr C19 97(100)
O2 C15 Cr C18 -173(100)
O2 C15 Cr P -6(100)
O3 C16 Cr C15 -15(3)
O3 C16 Cr C17 77(3)
O3 C16 Cr C19 -106(3)
O3 C16 Cr C18 -8(3)
O3 C16 Cr P 164(3)
O4 C17 Cr C15 -169(100)
O4 C17 Cr C16 104(8)
O4 C17 Cr C19 -16(9)
O4 C17 Cr C18 -83(8)
O4 C17 Cr P 15(8)
O6 C19 Cr C15 -1(6)
O6 C19 Cr C16 87(6)
O6 C19 Cr C17 -154(5)
O6 C19 Cr C18 -87(6)
O6 C19 Cr P 175(100)
O5 C18 Cr C15 9.4(12)
O5 C18 Cr C16 2.3(17)
O5 C18 Cr C17 -83.0(12)
O5 C18 Cr C19 100.2(12)
O5 C18 Cr P -169.6(12)
C4 C1 O1 P 120.13(15)
C2 C1 O1 P -131.09(15)
C1 O1 P C5 105.72(10)
C1 O1 P Cr -108.80(8)
C4 C1 P O1 -102.83(18)
C2 C1 P O1 103.6(2)
O1 C1 P C5 -91.96(9)
C4 C1 P C5 165.21(15)
C2 C1 P C5 11.7(2)
O1 C1 P Cr 103.24(8)
C4 C1 P Cr 0.41(19)
C2 C1 P Cr -153.12(17)
C9 C5 P O1 -164.03(11)
C6 C5 P O1 86.99(12)
C10 C5 P O1 -37.30(14)
C9 C5 P C1 -110.93(12)
C6 C5 P C1 140.08(11)
C10 C5 P C1 15.79(15)
C9 C5 P Cr 53.26(13)
C6 C5 P Cr -55.73(13)
C10 C5 P Cr 179.98(9)
C15 Cr P O1 32.0(8)
C16 Cr P O1 19.71(8)
C17 Cr P O1 110.26(7)
C19 Cr P O1 -71.53(7)
C18 Cr P O1 -161.22(7)
C15 Cr P C1 -27.3(8)
C16 Cr P C1 -39.61(9)
C17 Cr P C1 50.94(9)
C19 Cr P C1 -130.86(9)
C18 Cr P C1 139.45(9)
C15 Cr P C5 170.0(8)
C16 Cr P C5 157.73(9)
C17 Cr P C5 -111.72(8)
C19 Cr P C5 66.48(9)
C18 Cr P C5 -23.21(9)
