#------------------------------------------------------------------------------
#$Date: 2017-07-10 18:33:26 +0300 (Mon, 10 Jul 2017) $
#$Revision: 198601 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/00/39/2003901.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2003901
loop_
_publ_author_name
'Grehl, M.'
'Berlekamp, M.'
'Erker, G.'
_publ_section_title
;
 A Nine-Membered Metallacyclic Metalloxycarbene Vanadium Complex
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1772
_journal_page_last               1774
_journal_paper_doi               10.1107/S0108270195002435
_journal_volume                  51
_journal_year                    1995
_chemical_formula_moiety         'C31.5 H33 O5 V1 Zr1'
_chemical_formula_sum            'C31.5 H33 O5 V Zr'
_chemical_formula_weight         633.74
_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'
_atom_type_scat_source           IntTabIV
_cell_angle_alpha                90.
_cell_angle_beta                 101.44(1)
_cell_angle_gamma                90.
_cell_formula_units_Z            4
_cell_length_a                   8.311(1)
_cell_length_b                   17.111(1)
_cell_length_c                   20.500(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      20.82
_cell_measurement_theta_min      11.90
_cell_volume                     2857.4(5)
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       ω/2θ
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.014
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            8762
_diffrn_reflns_theta_max         30.42
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.73
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.88
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            'dark violet'
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_description       irregular
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.31
_refine_diff_density_max         0.40
_refine_diff_density_min         -0.40
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.268
_refine_ls_hydrogen_treatment    'H atoms in calculated positions'
_refine_ls_number_parameters     368
_refine_ls_number_reflns         8065
_refine_ls_R_factor_obs          0.061
_refine_ls_shift/esd_max         '< 0.001'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
' Weighting scheme based on measured e.s.d.'s'
_refine_ls_wR_factor_obs         0.091
_reflns_number_observed          6364
_reflns_number_total             8281
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            jz1002.cif
_cod_data_source_block           jz1002a
_cod_depositor_comments
;
 Marking atoms 'C(29)', 'C(30)', 'C(31)', 'C(32)', 'C(33)', 'C(34)', 'C(35)',
 'H(30)', 'H(31)', 'H(32)', 'H(33)', 'H(34)', 'H(35A)', 'H(35B)', 'H(35C)' as
 having the occupancy of 0.5 after consulting the original publication.

 Antanas Vaitkus,
 2017-07-05

 Changing the space group from '-P 2yb' to '-P 2yn' after consulting the
 original publication. All related space group information was changed
 accordingly.

 Antanas Vaitkus,
 2017-07-05

The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value '\y scan' was replaced with
the value 'psi-scan' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_original_cell_volume        2857.3(4)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C31.5 H33 O5 V1 Zr1'
_cod_database_code               2003901
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x+1/2,y+1/2,-z+1/2
3 -x,-y,-z
4 x+1/2,-y+1/2,z+1/2
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
Zr(1) .3140(1) .3359(1) .2375(1) .032(1) 1
V(1) .4971(1) .2086(1) .0440(1) .034(1) 1
O(1) .7277(2) .1886(1) .1786(1) .057(1) 1
O(2) .4101(3) .0488(1) .0944(1) .068(1) 1
O(3) .1290(3) .2202(2) .0455(1) .075(1) 1
O(4) .4003(2) .3115(1) .1510(1) .038(1) 1
O(5) .4419(2) .4231(1) .2758(1) .040(1) 1
C(1) .6386(3) .1964(1) .1281(1) .040(1) 1
C(2) .4418(3) .1085(2) .0739(1) .045(1) 1
C(3) .2663(3) .2160(2) .0450(1) .047(1) 1
C(4) .4754(3) .3073(1) .1023(1) .033(1) 1
C(5) .5658(3) .3834(1) .0917(1) .044(1) 1
C(6) .5239(3) .4502(1) .1321(1) .041(1) 1
C(7) .6198(3) .4789(2) .1853(1) .042(1) 1
C(8) .5615(3) .5336(1) .2321(1) .045(1) 1
C(9) .5354(3) .4913(1) .2952(1) .037(1) 1
C(10) .6959(3) .4684(2) .3428(2) .053(1) 1
C(11) .6610(4) .4727(2) .4132(2) .065(1) 1
C(12) .4839(4) .5012(2) .4064(1) .057(1) 1
C(13) .4479(3) .5417(2) .3389(1) .046(1) 1
C(14) .3016(4) .2508(2) .3357(2) .060(1) 1
C(15) .2687(4) .2004(2) .2806(2) .059(1) 1
C(16) .4116(4) .1934(2) .2549(2) .055(1) 1
C(17) .5329(4) .2398(2) .2941(2) .054(1) 1
C(18) .4657(4) .2734(2) .3447(1) .057(1) 1
C(19) .0645(4) .4107(2) .2538(2) .067(1) 1
C(20) .0109(3) .3343(2) .2392(2) .063(1) 1
C(21) .0228(3) .3184(2) .1735(2) .060(1) 1
C(22) .0799(3) .3858(2) .1474(2) .060(1) 1
C(23) .1047(4) .4428(2) .1962(2) .065(1) 1
C(24) .5333(4) .2808(2) -.0456(1) .050(1) 1
C(25) .6875(3) .2607(2) -.0086(1) .048(1) 1
C(26) .7030(4) .1792(2) -.0111(2) .053(1) 1
C(27) .5587(4) .1491(2) -.0492(2) .058(1) 1
C(28) .4532(4) .2111(2) -.0703(1) .057(1) 1
C(29) -.0432(10) .5330(4) .0251(4) .069(2) 0.5
C(30) -.1445(8) .4770(5) -.0112(4) .072(3) 0.5
C(31) -.0804(15) .4241(4) -.0507(3) .098(4) 0.5
C(32) .0849(17) .4271(5) -.0540(4) .138(11) 0.5
C(33) .1862(10) .4831(6) -.0177(5) .097(3) 0.5
C(34) .1222(9) .5361(4) .0219(4) .072(3) 0.5
C(35) -.1072(22) .5869(12) .0653(10) .119(7) 0.5
H(5A) .6832(3) .3742(1) .1029(1) .053 1
H(5B) .5380(3) .3975(1) .0450(1) .053 1
H(6) .4213(3) .4732(1) .1187(1) .049 1
H(7) .7297(3) .4642(2) .1940(1) .051 1
H(8A) .4596(3) .5579(1) .2101(1) .055 1
H(8B) .6425(3) .5746(1) .2444(1) .055 1
H(10A) .7285(3) .4159(2) .3332(2) .064 1
H(10B) .7833(3) .5042(2) .3381(2) .064 1
H(11A) .7360(4) .5089(2) .4401(2) .078 1
H(11B) .6749(4) .4216(2) .4341(2) .078 1
H(12A) .4100(4) .4575(2) .4074(1) .068 1
H(12B) .4740(4) .5372(2) .4419(1) .068 1
H(13A) .3308(3) .5434(2) .3210(1) .056 1
H(13B) .4908(3) .5946(2) .3423(1) .056 1
H(14) .2270(4) .2664(2) .3614(2) .072 1
H(15) .1690(4) .1759(2) .2641(2) .071 1
H(16) .4244(4) .1633(2) .2185(2) .066 1
H(17) .6394(4) .2470(2) .2876(2) .065 1
H(18) .5208(4) .3052(2) .3787(1) .069 1
H(19) .0720(4) .4356(2) .2946(2) .081 1
H(20) -.0259(3) .2999(2) .2682(2) .076 1
H(21) -.0024(3) .2712(2) .1514(2) .072 1
H(22) .0972(3) .3913(2) .1042(2) .072 1
H(23) .1415(4) .4935(5) .1917(2) .078 1
H(24) .4915(4) .3312(2) -.0526(1) .060 1
H(25) .7654(3) .2954(2) .0139(1) .058 1
H(26) .7937(4) .1502(2) .0092(2) .063 1
H(27) .5366(4) .0967(2) -.0593(2) .069 1
H(28) .3479(4) .2075(2) -.0960(1) .068 1
H(30) -.2551(8) .4749(7) -.0090(6) .086 0.5
H(31) -.1482(20) .3866(5) -.0750(4) .118 0.5
H(32) .1278(23) .3917(6) -.0805(6) .165 0.5
H(33) .2969(11) .4852(8) -.0199(7) .116 0.5
H(34) .1900(13) .5735(5) .0461(5) .086 0.5
H(35A) -.2011(71) .6125(39) .0393(14) .179 0.5
H(35B) -.0249(44) .6251(33) .0823(38) .179 0.5
H(35C) -.1391(101) .5598(14) .1017(26) .179 0.5
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
O(5) Zr(1) O(4) 104.41(7) yes
C(1) V(1) C(3) 115.93(11) yes
C(1) V(1) C(4) 71.24(9) yes
C(3) V(1) C(4) 75.12(10) yes
C(9) O(5) Zr(1) 172.3(2) yes
O(2) C(2) V(1) 177.5(3) yes
O(4) C(4) C(5) 112.9(2) yes
C(5) C(4) V(1) 120.1(2) yes
C(7) C(6) C(5) 125.3(2) yes
C(7) C(8) C(9) 111.4(2) yes
O(5) C(9) C(8) 108.2(2) yes
O(5) C(9) C(10) 109.1(2) yes
C(8) C(9) C(10) 113.9(2) yes
C(10) C(11) C(12) 106.8(2) yes
C(12) C(13) C(9) 104.2(2) yes
C(16) C(15) C(14) 108.1(3) yes
C(18) C(17) C(16) 108.1(3) yes
C(20) C(19) C(23) 107.9(3) yes
C(22) C(21) C(20) 107.7(3) yes
C(23) C(22) Zr(1) 74.3(2) yes
C(22) C(23) C(19) 107.8(3) yes
C(19) C(23) Zr(1) 72.5(2) yes
C(25) C(24) V(1) 71.5(2) yes
C(24) C(25) C(26) 107.8(3) yes
C(26) C(25) V(1) 72.8(2) yes
C(27) C(26) V(1) 73.3(2) yes
C(28) C(27) C(26) 108.1(3) yes
C(26) C(27) V(1) 71.4(2) yes
C(27) C(28) V(1) 72.9(2) yes
C(1) V(1) C(2) 75.79(11) yes
C(2) V(1) C(3) 75.61(12) yes
C(2) V(1) C(4) 119.17(10) yes
C(4) O(4) Zr(1) 168.2(2) yes
O(1) C(1) V(1) 178.4(2) yes
O(3) C(3) V(1) 179.8(3) yes
O(4) C(4) V(1) 126.9(2) yes
C(6) C(5) C(4) 113.3(2) yes
C(6) C(7) C(8) 123.3(2) yes
O(5) C(9) C(13) 109.4(2) yes
C(13) C(9) C(8) 113.1(2) yes
C(13) C(9) C(10) 103.0(2) yes
C(11) C(10) C(9) 106.5(2) yes
C(13) C(12) C(11) 103.9(2) yes
C(18) C(14) C(15) 107.9(3) yes
C(15) C(16) C(17) 107.7(3) yes
C(14) C(18) C(17) 108.2(3) yes
C(19) C(20) C(21) 108.0(3) yes
C(23) C(22) C(21) 108.6(3) yes
C(21) C(22) Zr(1) 73.4(2) yes
C(22) C(23) Zr(1) 74.2(2) yes
C(25) C(24) C(28) 107.7(3) yes
C(28) C(24) V(1) 72.8(2) yes
C(24) C(25) V(1) 72.7(2) yes
C(27) C(26) C(25) 108.3(3) yes
C(25) C(26) V(1) 71.3(2) yes
C(28) C(27) V(1) 72.0(2) yes
C(27) C(28) C(24) 108.1(3) yes
C(24) C(28) V(1) 71.4(2) yes
O(4) Zr(1) C(14) 130.07(9) no
O(4) Zr(1) C(19) 130.37(10) no
O(5) Zr(1) C(20) 118.58(10) no
C(14) Zr(1) C(20) 77.43(11) no
O(5) Zr(1) C(21) 134.66(10) no
C(14) Zr(1) C(21) 99.25(11) no
C(20) Zr(1) C(21) 32.09(10) no
O(4) Zr(1) C(15) 102.29(9) no
C(19) Zr(1) C(15) 103.63(12) no
C(21) Zr(1) C(15) 83.10(12) no
O(4) Zr(1) C(18) 117.13(9) no
C(19) Zr(1) C(18) 112.31(12) no
C(21) Zr(1) C(18) 131.13(11) no
O(5) Zr(1) C(22) 108.59(10) no
C(14) Zr(1) C(22) 129.07(11) no
C(20) Zr(1) C(22) 52.71(10) no
C(15) Zr(1) C(22) 114.45(11) no
O(5) Zr(1) C(23) 82.13(10) no
C(14) Zr(1) C(23) 123.38(11) no
C(20) Zr(1) C(23) 52.86(11) no
O(5) Zr(1) C(14) 103.48(10) no
O(5) Zr(1) C(19) 87.39(10) no
C(14) Zr(1) C(19) 91.30(12) no
O(4) Zr(1) C(20) 121.50(9) no
C(19) Zr(1) C(20) 32.10(11) no
O(4) Zr(1) C(21) 89.43(9) no
C(19) Zr(1) C(21) 53.16(11) no
O(5) Zr(1) C(15) 132.93(9) no
C(14) Zr(1) C(15) 32.35(10) no
C(20) Zr(1) C(15) 76.580(10) no
O(5) Zr(1) C(18) 80.41(9) no
C(14) Zr(1) C(18) 32.07(11) no
C(20) Zr(1) C(18) 107.950(10) no
C(15) Zr(1) C(18) 52.90(11) no
O(4) Zr(1) C(22) 78.03(9) no
C(19) Zr(1) C(22) 52.78(11) no
C(21) Zr(1) C(22) 31.82(10) no
C(18) Zr(1) C(22) 160.64(11) no
O(4) Zr(1) C(23) 100.88(10) no
C(19) Zr(1) C(23) 32.13(11) no
C(21) Zr(1) C(23) 52.69(12) no
C(15) Zr(1) C(23) 129.27(11) no
C(22) Zr(1) C(23) 31.48(11) no
O(4) Zr(1) C(17) 85.60(9) no
C(19) Zr(1) C(17) 143.01(11) no
C(21) Zr(1) C(17) 132.91(11) no
C(18) Zr(1) C(17) 31.78(9) no
C(23) Zr(1) C(17) 171.92(11) no
O(4) Zr(1) C(16) 77.04(8) no
C(19) Zr(1) C(16) 135.19(12) no
C(21) Zr(1) C(16) 101.69(11) no
C(18) Zr(1) C(16) 52.59(10) no
C(23) Zr(1) C(16) 154.37(11) no
C(1) V(1) C(25) 96.33(10) no
C(3) V(1) C(25) 140.31(12) no
C(1) V(1) C(24) 129.37(11) no
C(3) V(1) C(24) 105.26(11) no
C(25) V(1) C(24) 35.75(10) no
C(2) V(1) C(26) 102.31(11) no
C(4) V(1) C(26) 128.03(10) no
C(24) V(1) C(26) 59.33(10) no
C(2) V(1) C(28) 110.16(12) no
C(4) V(1) C(28) 123.46(11) no
C(24) V(1) C(28) 35.84(11) no
C(1) V(1) C(27) 120.30(12) no
C(3) V(1) C(27) 114.93(12) no
C(25) V(1) C(27) 59.35(10) no
C(26) V(1) C(27) 35.30(11) no
C(15) C(14) Zr(1) 75.1(2) no
C(16) C(15) Zr(1) 75.6(2) no
C(17) C(16) Zr(1) 73.4(2) no
C(18) C(17) Zr(1) 73.6(2) no
C(17) C(18) Zr(1) 74.6(2) no
C(20) C(19) Zr(1) 74.4(2) no
C(21) C(20) Zr(1) 74.2(2) no
C(22) C(21) Zr(1) 74.8(2) no
C(18) Zr(1) C(23) 141.00(11) no
O(5) Zr(1) C(17) 91.63(9) no
C(14) Zr(1) C(17) 53.05(11) no
C(20) Zr(1) C(17) 127.50(11) no
C(15) Zr(1) C(17) 52.72(11) no
C(22) Zr(1) C(17) 156.52(11) no
O(5) Zr(1) C(16) 123.34(9) no
C(14) Zr(1) C(16) 53.03(10) no
C(20) Zr(1) C(16) 106.00(11) no
C(15) Zr(1) C(16) 31.71(10) no
C(22) Zr(1) C(16) 126.33(11) no
C(17) Zr(1) C(16) 31.77(10) no
C(2) V(1) C(25) 137.91(11) no
C(4) V(1) C(25) 95.79(9) no
C(2) V(1) C(24) 145.46(11) no
C(4) V(1) C(24) 93.58(9) no
C(1) V(1) C(26) 92.03(11) no
C(3) V(1) C(26) 149.77(11) no
C(25) V(1) C(26) 35.88(10) no
C(1) V(1) C(28) 150.83(11) no
C(3) V(1) C(28) 92.99(12) no
C(25) V(1) C(28) 59.50(10) no
C(26) V(1) C(28) 58.87(11) no
C(2) V(1) C(27) 88.66(11) no
C(4) V(1) C(27) 152.17(10) no
C(24) V(1) C(27) 59.12(11) no
C(28) V(1) C(27) 35.08(12) no
C(18) C(14) Zr(1) 75.5(2) no
C(14) C(15) Zr(1) 72.5(2) no
C(15) C(16) Zr(1) 72.7(2) no
C(16) C(17) Zr(1) 74.8(2) no
C(14) C(18) Zr(1) 72.4(2) no
C(23) C(19) Zr(1) 75.3(2) no
C(19) C(20) Zr(1) 73.5(2) no
C(20) C(21) Zr(1) 73.7(2) no
C(30) C(29) C(35) 120.4(11) no
C(31) C(30) C(29) 120.0 no
C(33) C(32) C(31) 120.0 no
C(33) C(34) C(29) 120.0 no
C(30) C(29) C(34) 120.0 no
C(34) C(29) C(35) 119.6(11) no
C(32) C(31) C(30) 120.0 no
C(32) C(33) C(34) 120.0 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Zr(1) O(5) 1.908(2) yes
Zr(1) C(14) 2.503(3) yes
Zr(1) C(20) 2.526(3) yes
Zr(1) C(15) 2.536(3) yes
Zr(1) C(22) 2.549(3) yes
Zr(1) C(17) 2.555(3) yes
V(1) C(1) 1.896(3) yes
V(1) C(3) 1.926(3) yes
V(1) C(25) 2.266(2) yes
V(1) C(26) 2.285(3) yes
V(1) C(27) 2.311(3) yes
O(2) C(2) 1.154(3) yes
O(4) C(4) 1.280(2) yes
C(4) C(5) 1.540(3) yes
C(6) C(7) 1.312(3) yes
C(8) C(9) 1.536(4) yes
C(9) C(10) 1.539(3) yes
C(11) C(12) 1.530(4) yes
C(14) C(18) 1.394(5) yes
C(15) C(16) 1.396(4) yes
C(17) C(18) 1.395(4) yes
C(19) C(23) 1.402(5) yes
C(21) C(22) 1.393(5) yes
C(24) C(25) 1.396(4) yes
C(25) C(26) 1.402(4) yes
C(27) C(28) 1.390(5) yes
Zr(1) O(4) 2.084(2) yes
Zr(1) C(19) 2.514(3) yes
Zr(1) C(21) 2.531(3) yes
Zr(1) C(18) 2.542(3) yes
Zr(1) C(23) 2.550(3) yes
Zr(1) C(16) 2.572(3) yes
V(1) C(2) 1.906(3) yes
V(1) C(4) 2.096(2) yes
V(1) C(24) 2.282(3) yes
V(1) C(28) 2.300(3) yes
O(1) C(1) 1.154(3) yes
O(3) C(3) 1.145(3) yes
O(5) C(9) 1.415(3) yes
C(5) C(6) 1.493(3) yes
C(7) C(8) 1.488(3) yes
C(9) C(13) 1.527(3) yes
C(10) C(11) 1.528(4) yes
C(12) C(13) 1.523(4) yes
C(14) C(15) 1.404(4) yes
C(16) C(17) 1.404(4) yes
C(19) C(20) 1.393(5) yes
C(20) C(21) 1.398(4) yes
C(22) C(23) 1.383(5) yes
C(24) C(28) 1.410(4) yes
C(26) C(27) 1.394(4) yes
C(27) C(28) 1.390(5) no
C(29) C(34) 1.39 no
C(30) C(31) 1.39 no
C(32) C(33) 1.39 no
C(29) C(30) 1.39 no
C(29) C(35) 1.41(2) no
C(31) C(32) 1.39 no
C(33) C(34) 1.39 no
