#------------------------------------------------------------------------------
#$Date: 2025-08-21 14:03:24 +0200 (Thu 21 de Aug de 2025) $
#$Revision: 301848 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/08/7020859.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_7020859
loop_
_publ_author_name
'Xing, Na'
'Shan, Hui'
'Tian, Xing'
'Yao, Qiang'
'Xu, Li-Ting'
'Xing, Yong-Heng'
'Shi, Zhan'
_publ_section_title
;
 Two new scorpionate oxomolybdenum(VI)-poly(pyrazolyl)borate complexes:
 synthesis, structure, and catalytic performance in the oxidation of
 cyclohexane.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              359
_journal_page_last               363
_journal_paper_doi               10.1039/c2dt32184j
_journal_volume                  42
_journal_year                    2013
_chemical_formula_sum            'C18 H14 B2 I6 Mo2 N12 O5'
_chemical_formula_weight         1453.31
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.9610(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.0143(7)
_cell_length_b                   13.1374(5)
_cell_length_c                   18.3143(8)
_cell_measurement_reflns_used    4512
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.09
_cell_measurement_theta_min      2.38
_cell_volume                     3598.1(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Bruker AXS SMART APEX II CCD'
_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  0.0231
_diffrn_reflns_av_sigmaI/netI    0.0282
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            11115
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    5.893
_exptl_absorpt_correction_T_max  0.9838
_exptl_absorpt_correction_T_min  0.7501
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.683
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2632
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.168
_refine_diff_density_min         -2.156
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         4337
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0367
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0305P)²+24.5820P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0816
_refine_ls_wR_factor_ref         0.0872
_reflns_number_gt                3540
_reflns_number_total             4337
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt32184j.txt
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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      C2/c
_cod_database_code               7020859
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_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
I2A I 0.1055(2) 0.6671(4) 0.55497(16) 0.0747(7) Uani 0.599(17) 1 d P A 1
I3A I 0.6907(3) 1.0101(3) 0.8722(3) 0.0887(10) Uani 0.599(17) 1 d P A 1
I2B I 0.1129(5) 0.6931(9) 0.5588(3) 0.1056(17) Uani 0.401(17) 1 d P A 2
I3B I 0.6671(9) 1.0218(5) 0.8533(6) 0.107(2) Uani 0.401(17) 1 d P A 2
H7 H 0.323(3) 0.898(4) 0.846(3) 0.041(14) Uiso 1 1 d . . .
I1 I 0.39138(3) 0.67666(4) 1.14691(2) 0.06788(16) Uani 1 1 d . . .
C1 C 0.3556(3) 0.7737(4) 0.9836(3) 0.0415(11) Uani 1 1 d . . .
H1 H 0.3288 0.8319 0.9939 0.050 Uiso 1 1 calc R . .
C2 C 0.3862(3) 0.6928(4) 1.0332(3) 0.0418(11) Uani 1 1 d . . .
C3 C 0.4207(3) 0.6250(4) 0.9936(3) 0.0404(11) Uani 1 1 d . . .
H2 H 0.4463 0.5625 1.0129 0.048 Uiso 1 1 calc R . .
C4 C 0.2277(4) 0.7776(5) 0.7119(3) 0.0464(13) Uani 1 1 d . A .
H3 H 0.1919 0.8351 0.7054 0.056 Uiso 1 1 calc R . .
C5 C 0.2114(4) 0.6962(5) 0.6620(3) 0.0502(14) Uani 1 1 d . . .
C6 C 0.2809(3) 0.6280(4) 0.6951(3) 0.0404(11) Uani 1 1 d . A .
H4 H 0.2872 0.5650 0.6744 0.049 Uiso 1 1 calc R . .
C7 C 0.4936(5) 0.9362(4) 0.8491(3) 0.0557(15) Uani 1 1 d . A .
H5 H 0.4702 1.0008 0.8499 0.067 Uiso 1 1 calc R . .
C8 C 0.5782(4) 0.9156(4) 0.8535(3) 0.0512(14) Uani 1 1 d . . .
C9 C 0.5835(4) 0.8099(4) 0.8511(3) 0.0416(11) Uani 1 1 d . A .
H6 H 0.6342 0.7732 0.8538 0.050 Uiso 1 1 calc R . .
O1 O 0.5697(2) 0.5839(3) 0.91437(19) 0.0430(8) Uani 1 1 d . A .
O2 O 0.4154(2) 0.4871(3) 0.8384(2) 0.0468(9) Uani 1 1 d . A .
O3 O 0.5000 0.5923(3) 0.7500 0.0338(9) Uani 1 2 d S . .
N1 N 0.3710(3) 0.7546(3) 0.9175(2) 0.0370(9) Uani 1 1 d . . .
N2 N 0.4117(3) 0.6627(3) 0.9237(2) 0.0357(9) Uani 1 1 d . A .
N3 N 0.3046(3) 0.7598(3) 0.7720(2) 0.0383(9) Uani 1 1 d . . .
N4 N 0.3378(3) 0.6682(3) 0.7620(2) 0.0343(8) Uani 1 1 d . A .
N5 N 0.4489(3) 0.8477(3) 0.8433(2) 0.0410(9) Uani 1 1 d . . .
N6 N 0.5048(3) 0.7695(3) 0.8444(2) 0.0344(8) Uani 1 1 d . A .
B B 0.3555(4) 0.8230(4) 0.8449(3) 0.0404(13) Uani 1 1 d . A .
Mo Mo 0.47010(2) 0.59871(3) 0.84042(2) 0.02737(10) 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'
B B 0.0013 0.0007 '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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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
N1 C1 C2 108.5(4) .
N1 C1 H1 125.8 .
C2 C1 H1 125.8 .
C1 C2 C3 105.5(4) .
C1 C2 I1 128.7(4) .
C3 C2 I1 125.6(4) .
N2 C3 C2 109.8(4) .
N2 C3 H2 125.1 .
C2 C3 H2 125.1 .
N3 C4 C5 108.1(5) .
N3 C4 H3 126.0 .
C5 C4 H3 126.0 .
C4 C5 C6 106.3(5) .
C4 C5 I2B 123.3(5) .
C6 C5 I2B 130.0(5) .
C4 C5 I2A 131.0(4) .
C6 C5 I2A 122.6(5) .
I2B C5 I2A 9.3(4) .
N4 C6 C5 108.6(5) .
N4 C6 H4 125.7 .
C5 C6 H4 125.7 .
N5 C7 C8 108.9(5) .
N5 C7 H5 125.6 .
C8 C7 H5 125.6 .
C7 C8 C9 105.6(5) .
C7 C8 I3B 124.0(6) .
C9 C8 I3B 130.2(6) .
C7 C8 I3A 132.0(4) .
C9 C8 I3A 122.2(5) .
I3B C8 I3A 11.8(4) .
N6 C9 C8 109.5(5) .
N6 C9 H6 125.2 .
C8 C9 H6 125.2 .
Mo O3 Mo 174.9(3) 2_656
C1 N1 N2 109.1(4) .
C1 N1 B 129.8(4) .
N2 N1 B 120.9(4) .
C3 N2 N1 107.2(4) .
C3 N2 Mo 126.3(3) .
N1 N2 Mo 125.9(3) .
C4 N3 N4 109.3(4) .
C4 N3 B 131.5(4) .
N4 N3 B 119.1(4) .
C6 N4 N3 107.6(4) .
C6 N4 Mo 126.1(3) .
N3 N4 Mo 126.2(3) .
C7 N5 N6 108.8(4) .
C7 N5 B 132.2(5) .
N6 N5 B 118.6(4) .
C9 N6 N5 107.2(4) .
C9 N6 Mo 126.9(3) .
N5 N6 Mo 125.8(3) .
N3 B N5 108.3(4) .
N3 B N1 107.7(4) .
N5 B N1 106.3(4) .
N3 B H7 112(3) .
N5 B H7 106(3) .
N1 B H7 116(3) .
O1 Mo O2 104.39(18) .
O1 Mo O3 103.58(12) .
O2 Mo O3 103.46(18) .
O1 Mo N2 90.11(16) .
O2 Mo N2 90.09(16) .
O3 Mo N2 157.41(15) .
O1 Mo N4 161.04(16) .
O2 Mo N4 88.62(16) .
O3 Mo N4 86.29(11) .
N2 Mo N4 75.91(14) .
O1 Mo N6 86.51(16) .
O2 Mo N6 162.84(16) .
O3 Mo N6 86.39(16) .
N2 Mo N6 76.46(14) .
N4 Mo N6 77.89(14) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
I2A C5 2.119(6) .
I3A C8 2.113(6) .
I2B C5 1.983(8) .
I3B C8 1.994(8) .
I1 C2 2.065(5) .
C1 N1 1.342(6) .
C1 C2 1.369(7) .
C1 H1 0.9300 .
C2 C3 1.382(7) .
C3 N2 1.332(6) .
C3 H2 0.9300 .
C4 N3 1.346(6) .
C4 C5 1.369(8) .
C4 H3 0.9300 .
C5 C6 1.388(7) .
C6 N4 1.345(6) .
C6 H4 0.9300 .
C7 N5 1.350(7) .
C7 C8 1.354(9) .
C7 H5 0.9300 .
C8 C9 1.393(7) .
C9 N6 1.331(6) .
C9 H6 0.9300 .
O1 Mo 1.695(3) .
O2 Mo 1.701(3) .
O3 Mo 1.8830(4) 2_656
O3 Mo 1.8830(4) .
N1 N2 1.357(5) .
N1 B 1.548(6) .
N2 Mo 2.221(4) .
N3 N4 1.355(5) .
N3 B 1.536(7) .
N4 Mo 2.283(4) .
N5 N6 1.358(5) .
N5 B 1.542(8) .
N6 Mo 2.306(4) .
B H7 1.12(5) .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139159177
