#------------------------------------------------------------------------------
#$Date: 2019-11-17 13:04:48 +0200 (Sun, 17 Nov 2019) $
#$Revision: 230037 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/55/7045549.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_7045549
loop_
_publ_author_name
'Jurić, Marijana'
'Androš Dubraja, Lidija'
'Popović, Jasminka'
'Molčanov, Krešimir'
'Torić, Filip'
'Pajić, Damir'
'Lončarić, Ivor'
_publ_section_title
;
 From a square core to square opening: structural diversity and magnetic
 properties of the oxo-bridged [CrIIINbV] complexes.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4183
_journal_page_last               4190
_journal_paper_doi               10.1039/c7dt04724j
_journal_volume                  47
_journal_year                    2018
_chemical_formula_sum            'C38 H34 Cr2 N6 Nb2 O26'
_chemical_formula_weight         1280.54
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2018-02-01 deposited with the CCDC.
2018-02-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.766(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.0343(9)
_cell_length_b                   17.4862(14)
_cell_length_c                   11.9713(7)
_cell_measurement_reflns_used    9891
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      54.91
_cell_measurement_theta_min      4.664
_cell_volume                     2309.6(3)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'Bruker Instrument Service v4.2.2'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'Sir 92'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
'D8 Venture Bruker with double microsource Ag-Mo'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1147
_diffrn_reflns_av_unetI/netI     0.0530
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            51049
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.547
_diffrn_reflns_theta_min         2.329
_exptl_absorpt_coefficient_mu    1.043
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.736
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.841
_exptl_crystal_description       stick
_exptl_crystal_F_000             1284
_exptl_crystal_size_max          0.269
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.069
_refine_diff_density_max         0.564
_refine_diff_density_min         -0.778
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         5310
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0596
_refine_ls_R_factor_gt           0.0372
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0239P)²+4.7729P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0769
_refine_ls_wR_factor_ref         0.0851
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4154
_reflns_number_total             5310
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt04724j2.cif
_cod_data_source_block           CrtrpyNbox-2
_cod_depositor_comments
'Adding full bibliography for 7045548--7045550.cif.'
_cod_database_code               7045549
_shelx_shelxl_version_number     2017/1
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
C1 C 0.6943(3) -0.08812(18) 0.7030(3) 0.0188(7) Uani 1 1 d . .
H1 H 0.701667 -0.038165 0.677253 0.023 Uiso 1 1 calc R U
C2 C 0.7139(3) -0.1026(2) 0.8154(3) 0.0256(8) Uani 1 1 d . .
H2 H 0.731794 -0.062961 0.864737 0.031 Uiso 1 1 calc R U
C3 C 0.7065(3) -0.1776(2) 0.8532(3) 0.0289(8) Uani 1 1 d . .
H3 H 0.721113 -0.188926 0.928072 0.035 Uiso 1 1 calc R U
C4 C 0.6771(3) -0.2351(2) 0.7786(3) 0.0256(8) Uani 1 1 d . .
H4 H 0.672104 -0.285569 0.802522 0.031 Uiso 1 1 calc R U
C5 C 0.6551(3) -0.21649(18) 0.6673(3) 0.0162(6) Uani 1 1 d . .
C6 C 0.6167(3) -0.27258(18) 0.5810(3) 0.0176(7) Uani 1 1 d . .
C7 C 0.6042(4) -0.3510(2) 0.5946(3) 0.0287(8) Uani 1 1 d . .
H7 H 0.619934 -0.374140 0.663228 0.034 Uiso 1 1 calc R U
C8 C 0.5677(4) -0.3938(2) 0.5030(3) 0.0336(9) Uani 1 1 d . .
H8 H 0.559973 -0.446535 0.510378 0.040 Uiso 1 1 calc R U
C9 C 0.5424(4) -0.36016(19) 0.4007(3) 0.0272(8) Uani 1 1 d . .
H9 H 0.517387 -0.389364 0.339648 0.033 Uiso 1 1 calc R U
C10 C 0.5554(3) -0.28141(18) 0.3921(3) 0.0180(7) Uani 1 1 d . .
C11 C 0.5352(3) -0.23394(19) 0.2918(3) 0.0183(7) Uani 1 1 d . .
C12 C 0.4855(3) -0.2607(2) 0.1926(3) 0.0255(8) Uani 1 1 d . .
H12 H 0.460810 -0.311412 0.186068 0.031 Uiso 1 1 calc R U
C13 C 0.4730(4) -0.2112(2) 0.1036(3) 0.0316(9) Uani 1 1 d . .
H13 H 0.438719 -0.228223 0.036728 0.038 Uiso 1 1 calc R U
C14 C 0.5111(4) -0.1363(2) 0.1136(3) 0.0294(8) Uani 1 1 d . .
H14 H 0.505548 -0.102915 0.053236 0.035 Uiso 1 1 calc R U
C15 C 0.5582(3) -0.1118(2) 0.2161(3) 0.0226(7) Uani 1 1 d . .
H15 H 0.581912 -0.061080 0.224406 0.027 Uiso 1 1 calc R U
C16 C 0.6790(3) 0.22485(18) 0.3104(3) 0.0158(6) Uani 1 1 d . .
C17 C 0.6482(3) 0.15894(18) 0.2271(3) 0.0173(7) Uani 1 1 d . .
C18 C 0.9481(3) 0.07902(17) 0.4521(3) 0.0151(6) Uani 1 1 d . .
C19 C 0.9020(3) 0.09283(17) 0.5714(3) 0.0165(7) Uani 1 1 d . .
N1 N 0.6652(2) -0.14316(14) 0.6298(2) 0.0137(5) Uani 1 1 d . .
N2 N 0.5927(2) -0.24027(14) 0.4815(2) 0.0148(5) Uani 1 1 d . .
N3 N 0.5702(2) -0.15953(15) 0.3028(2) 0.0167(6) Uani 1 1 d . .
O1 O 0.5357(2) 0.10236(12) 0.50429(18) 0.0149(5) Uani 1 1 d . .
O2 O 0.6690(2) -0.02450(12) 0.43725(18) 0.0151(4) Uani 1 1 d . .
O3 O 0.7037(2) 0.20095(12) 0.40866(18) 0.0174(5) Uani 1 1 d . .
O4 O 0.6776(2) 0.29136(13) 0.27812(19) 0.0225(5) Uani 1 1 d . .
O5 O 0.6389(3) 0.16959(14) 0.12786(19) 0.0303(6) Uani 1 1 d . .
O6 O 0.6341(2) 0.09264(12) 0.27569(18) 0.0171(5) Uani 1 1 d . .
O7 O 0.86285(19) 0.07293(12) 0.37843(17) 0.0157(5) Uani 1 1 d . .
O8 O 1.0575(2) 0.07632(13) 0.43533(19) 0.0200(5) Uani 1 1 d . .
O9 O 0.9713(2) 0.10388(15) 0.6486(2) 0.0266(6) Uani 1 1 d . .
O10 O 0.7833(2) 0.09369(12) 0.57947(18) 0.0157(5) Uani 1 1 d . .
O11 O 0.7969(2) -0.15997(12) 0.43071(18) 0.0157(5) Uani 1 1 d D .
H11A H 0.806(3) -0.1767(19) 0.3646(14) 0.024 Uiso 1 1 d D U
H11B H 0.848(3) -0.1284(17) 0.456(3) 0.024 Uiso 1 1 d D U
O12 O 0.6812(3) 0.01334(18) 0.0283(3) 0.0488(8) Uani 1 1 d D .
H12A H 0.653(5) 0.0554(18) 0.054(4) 0.073 Uiso 1 1 d D U
H12B H 0.732(4) -0.012(2) 0.070(3) 0.073 Uiso 1 1 d D U
O13 O 0.8579(3) -0.03982(18) 0.1780(3) 0.0456(8) Uani 1 1 d D .
H13A H 0.877(4) -0.0160(19) 0.238(2) 0.068 Uiso 1 1 d D U
H13B H 0.854(5) -0.0885(7) 0.172(4) 0.068 Uiso 1 1 d D U
Cr1 Cr 0.62702(5) -0.12933(3) 0.46060(4) 0.01045(11) Uani 1 1 d . .
Nb1 Nb 0.67623(3) 0.07792(2) 0.44096(2) 0.01119(8) 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'
N N 0.0061 0.0033 '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'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 '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
N1 C1 C2 122.6(3) . .
C1 C2 C3 118.7(3) . .
C4 C3 C2 119.4(3) . .
C3 C4 C5 119.1(3) . .
N1 C5 C4 121.4(3) . .
N1 C5 C6 114.7(3) . .
C4 C5 C6 123.9(3) . .
N2 C6 C7 120.1(3) . .
N2 C6 C5 113.0(3) . .
C7 C6 C5 126.9(3) . .
C8 C7 C6 118.1(3) . .
C7 C8 C9 121.7(3) . .
C8 C9 C10 117.9(3) . .
N2 C10 C9 120.0(3) . .
N2 C10 C11 112.8(3) . .
C9 C10 C11 127.2(3) . .
N3 C11 C12 121.0(3) . .
N3 C11 C10 114.8(3) . .
C12 C11 C10 124.2(3) . .
C13 C12 C11 119.0(3) . .
C12 C13 C14 120.2(3) . .
C13 C14 C15 118.5(3) . .
N3 C15 C14 121.6(3) . .
O4 C16 O3 127.1(3) . .
O4 C16 C17 119.9(3) . .
O3 C16 C17 113.0(3) . .
O5 C17 O6 124.5(3) . .
O5 C17 C16 122.1(3) . .
O6 C17 C16 113.5(3) . .
O8 C18 O7 126.7(3) . .
O8 C18 C19 119.6(3) . .
O7 C18 C19 113.7(3) . .
O9 C19 O10 124.2(3) . .
O9 C19 C18 121.5(3) . .
O10 C19 C18 114.3(3) . .
C1 N1 C5 118.8(3) . .
C1 N1 Cr1 126.8(2) . .
C5 N1 Cr1 114.4(2) . .
C6 N2 C10 122.3(3) . .
C6 N2 Cr1 119.1(2) . .
C10 N2 Cr1 118.4(2) . .
C15 N3 C11 119.7(3) . .
C15 N3 Cr1 125.5(2) . .
C11 N3 Cr1 114.7(2) . .
Nb1 O1 Cr1 167.61(13) . 3_656
Nb1 O2 Cr1 164.72(14) . .
C16 O3 Nb1 116.93(19) . .
C17 O6 Nb1 121.0(2) . .
C18 O7 Nb1 116.28(19) . .
C19 O10 Nb1 120.31(19) . .
O1 Cr1 O2 91.47(9) 3_656 .
O1 Cr1 O11 177.36(10) 3_656 .
O2 Cr1 O11 90.08(9) . .
O1 Cr1 N2 91.83(10) 3_656 .
O2 Cr1 N2 176.67(10) . .
O11 Cr1 N2 86.64(10) . .
O1 Cr1 N3 89.39(10) 3_656 .
O2 Cr1 N3 100.59(10) . .
O11 Cr1 N3 92.43(10) . .
N2 Cr1 N3 78.99(11) . .
O1 Cr1 N1 89.60(10) 3_656 .
O2 Cr1 N1 101.99(10) . .
O11 Cr1 N1 87.99(10) . .
N2 Cr1 N1 78.49(10) . .
N3 Cr1 N1 157.41(11) . .
O1 Nb1 O2 102.16(10) . .
O1 Nb1 O10 96.84(9) . .
O2 Nb1 O10 100.38(9) . .
O1 Nb1 O6 101.14(9) . .
O2 Nb1 O6 95.30(9) . .
O10 Nb1 O6 153.04(9) . .
O1 Nb1 O7 166.99(9) . .
O2 Nb1 O7 89.64(9) . .
O10 Nb1 O7 75.39(8) . .
O6 Nb1 O7 82.96(9) . .
O1 Nb1 O3 87.90(9) . .
O2 Nb1 O3 167.20(9) . .
O10 Nb1 O3 86.06(8) . .
O6 Nb1 O3 74.79(8) . .
O7 Nb1 O3 81.24(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.338(4) .
C1 C2 1.384(5) .
C2 C3 1.390(5) .
C3 C4 1.380(5) .
C4 C5 1.390(5) .
C5 N1 1.363(4) .
C5 C6 1.482(5) .
C6 N2 1.341(4) .
C6 C7 1.389(5) .
C7 C8 1.382(5) .
C8 C9 1.384(5) .
C9 C10 1.389(5) .
C10 N2 1.350(4) .
C10 C11 1.474(5) .
C11 N3 1.363(4) .
C11 C12 1.383(4) .
C12 C13 1.379(5) .
C13 C14 1.380(5) .
C14 C15 1.394(5) .
C15 N3 1.337(4) .
C16 O4 1.226(4) .
C16 O3 1.275(4) .
C16 C17 1.558(4) .
C17 O5 1.206(4) .
C17 O6 1.307(4) .
C18 O8 1.228(4) .
C18 O7 1.285(4) .
C18 C19 1.541(4) .
C19 O9 1.208(4) .
C19 O10 1.315(4) .
N1 Cr1 2.077(3) .
N2 Cr1 1.993(3) .
N3 Cr1 2.052(3) .
O1 Nb1 1.787(2) .
O1 Cr1 1.909(2) 3_656
O2 Nb1 1.793(2) .
O2 Cr1 1.912(2) .
O3 Nb1 2.207(2) .
O6 Nb1 2.043(2) .
O7 Nb1 2.202(2) .
O10 Nb1 2.042(2) .
O11 Cr1 1.987(2) .
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
_geom_torsion_site_symmetry_1
N1 C1 C2 C3 1.9(5) .
C1 C2 C3 C4 -1.5(6) .
C2 C3 C4 C5 -0.3(6) .
C3 C4 C5 N1 1.8(5) .
C3 C4 C5 C6 -176.7(3) .
N1 C5 C6 N2 -3.1(4) .
C4 C5 C6 N2 175.5(3) .
N1 C5 C6 C7 177.1(3) .
C4 C5 C6 C7 -4.3(6) .
N2 C6 C7 C8 0.5(5) .
C5 C6 C7 C8 -179.7(3) .
C6 C7 C8 C9 -0.9(6) .
C7 C8 C9 C10 0.4(6) .
C8 C9 C10 N2 0.5(5) .
C8 C9 C10 C11 179.1(3) .
N2 C10 C11 N3 7.0(4) .
C9 C10 C11 N3 -171.6(3) .
N2 C10 C11 C12 -173.3(3) .
C9 C10 C11 C12 8.1(6) .
N3 C11 C12 C13 0.9(5) .
C10 C11 C12 C13 -178.8(3) .
C11 C12 C13 C14 0.8(6) .
C12 C13 C14 C15 -2.2(6) .
C13 C14 C15 N3 1.9(6) .
O4 C16 C17 O5 10.5(5) .
O3 C16 C17 O5 -169.6(3) .
O4 C16 C17 O6 -169.7(3) .
O3 C16 C17 O6 10.2(4) .
O8 C18 C19 O9 2.7(5) .
O7 C18 C19 O9 -175.9(3) .
O8 C18 C19 O10 -179.2(3) .
O7 C18 C19 O10 2.1(4) .
C2 C1 N1 C5 -0.4(5) .
C2 C1 N1 Cr1 177.6(3) .
C4 C5 N1 C1 -1.5(5) .
C6 C5 N1 C1 177.2(3) .
C4 C5 N1 Cr1 -179.7(3) .
C6 C5 N1 Cr1 -1.1(3) .
C7 C6 N2 C10 0.4(5) .
C5 C6 N2 C10 -179.4(3) .
C7 C6 N2 Cr1 -174.0(3) .
C5 C6 N2 Cr1 6.1(4) .
C9 C10 N2 C6 -0.9(5) .
C11 C10 N2 C6 -179.7(3) .
C9 C10 N2 Cr1 173.5(3) .
C11 C10 N2 Cr1 -5.2(4) .
C14 C15 N3 C11 -0.3(5) .
C14 C15 N3 Cr1 -175.6(3) .
C12 C11 N3 C15 -1.1(5) .
C10 C11 N3 C15 178.6(3) .
C12 C11 N3 Cr1 174.7(3) .
C10 C11 N3 Cr1 -5.6(4) .
O4 C16 O3 Nb1 173.0(3) .
C17 C16 O3 Nb1 -7.0(3) .
O5 C17 O6 Nb1 170.9(3) .
C16 C17 O6 Nb1 -9.0(4) .
O8 C18 O7 Nb1 178.6(3) .
C19 C18 O7 Nb1 -2.9(3) .
O9 C19 O10 Nb1 177.8(2) .
C18 C19 O10 Nb1 -0.2(3) .
Cr1 O1 Nb1 O2 -91.3(6) 3_656
Cr1 O1 Nb1 O10 166.5(6) 3_656
Cr1 O1 Nb1 O6 6.7(6) 3_656
Cr1 O1 Nb1 O7 114.0(6) 3_656
Cr1 O1 Nb1 O3 80.8(6) 3_656
Cr1 O2 Nb1 O1 -14.8(5) .
Cr1 O2 Nb1 O10 84.6(5) .
Cr1 O2 Nb1 O6 -117.4(5) .
Cr1 O2 Nb1 O7 159.7(5) .
Cr1 O2 Nb1 O3 -156.0(4) .
