#------------------------------------------------------------------------------
#$Date: 2025-08-21 02:27:06 +0300 (Thu, 21 Aug 2025) $
#$Revision: 301840 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/28/4342859.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_4342859
loop_
_publ_author_name
'Chatterjee, Ipsita'
'Saha Chowdhury, Nabanita'
'Ghosh, Pradip'
'Goswami, Sreebrata'
_publ_section_title
;
 Octacoordinated Dioxo-Molybdenum Complex via Formal Oxidative Addition of
 Molecular Oxygen. Studies of Chemical Reactions Between M(CO)6 (M = Cr,
 Mo) and 2,4-Di-tert-butyl-6-(pyridin-2-ylazo)-phenol.
;
_journal_issue                   11
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5257
_journal_page_last               5265
_journal_paper_doi               10.1021/acs.inorgchem.5b00218
_journal_volume                  54
_journal_year                    2015
_chemical_formula_sum            'C38 H48 Cr N6 O2'
_chemical_formula_weight         672.82
_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                 113.908(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.210(3)
_cell_length_b                   15.258(2)
_cell_length_c                   17.196(3)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.8
_cell_measurement_theta_min      1.8
_cell_volume                     4367.9(12)
_computing_cell_refinement       'Bruker APEX-2'
_computing_data_collection       'Bruker APEX-2'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    ORTEP-III
_computing_publication_material  'WinGX v1.70.01'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0437
_diffrn_reflns_av_sigmaI/netI    0.0273
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22665
_diffrn_reflns_theta_full        23.77
_diffrn_reflns_theta_max         23.77
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    0.296
_exptl_absorpt_correction_T_max  0.9767
_exptl_absorpt_correction_T_min  0.9542
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.023
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       palate
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.180
_refine_diff_density_min         -0.230
_refine_diff_density_rms         0.034
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         3330
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0371
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0659P)²+0.8228P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1050
_refine_ls_wR_factor_ref         0.1113
_reflns_number_gt                2749
_reflns_number_total             3330
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b00218_si_002.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'EMPIRICAL' changed to
'empirical' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 4342858--4342860.cif.
;
_cod_original_cell_volume        4367.8(12)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4342859
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
Cr1 Cr 0.0000 0.11100(3) 0.7500 0.04118(18) Uani 1 2 d S
O1 O 0.01660(8) 0.20157(8) 0.67741(9) 0.0464(4) Uani 1 1 d .
N1 N 0.03358(11) 0.01861(10) 0.84431(11) 0.0464(4) Uani 1 1 d .
N3 N 0.11591(10) 0.09927(10) 0.78513(10) 0.0421(4) Uani 1 1 d .
N2 N 0.16084(10) 0.04217(11) 0.84260(11) 0.0521(5) Uani 1 1 d .
C10 C 0.11909(12) 0.27552(12) 0.64570(12) 0.0421(5) Uani 1 1 d .
C6 C 0.14907(11) 0.15076(12) 0.74201(12) 0.0406(5) Uani 1 1 d .
C7 C 0.22898(12) 0.14787(13) 0.75092(13) 0.0457(5) Uani 1 1 d .
H7 H 0.2643 0.1065 0.7862 0.055 Uiso 1 1 calc R
C11 C 0.09145(11) 0.20987(12) 0.68637(12) 0.0404(5) Uani 1 1 d .
C5 C 0.11374(13) 0.00013(13) 0.87632(13) 0.0484(5) Uani 1 1 d .
C8 C 0.25438(12) 0.20661(13) 0.70713(12) 0.0454(5) Uani 1 1 d .
C16 C 0.06314(13) 0.34900(13) 0.59473(13) 0.0509(5) Uani 1 1 d .
C9 C 0.19838(12) 0.27009(13) 0.65719(12) 0.0461(5) Uani 1 1 d .
H9 H 0.2167 0.3117 0.6298 0.055 Uiso 1 1 calc R
C2 C 0.02010(18) -0.08189(16) 0.94428(16) 0.0664(7) Uani 1 1 d .
H2 H -0.0129 -0.1093 0.9664 0.080 Uiso 1 1 calc R
C1 C -0.01156(15) -0.02326(14) 0.87852(15) 0.0576(6) Uani 1 1 d .
H1 H -0.0664 -0.0119 0.8566 0.069 Uiso 1 1 calc R
C4 C 0.14834(16) -0.05860(16) 0.94369(15) 0.0665(7) Uani 1 1 d .
H4 H 0.2032 -0.0697 0.9656 0.080 Uiso 1 1 calc R
C12 C 0.34033(12) 0.20770(16) 0.71193(14) 0.0566(6) Uani 1 1 d .
C19 C 0.02864(16) 0.39635(14) 0.65138(16) 0.0655(7) Uani 1 1 d .
H19A H -0.0065 0.4425 0.6196 0.098 Uiso 1 1 calc R
H19B H 0.0718 0.4207 0.7000 0.098 Uiso 1 1 calc R
H19C H -0.0009 0.3554 0.6700 0.098 Uiso 1 1 calc R
C17 C 0.10773(17) 0.41722(17) 0.56404(18) 0.0802(8) Uani 1 1 d .
H17A H 0.0709 0.4623 0.5325 0.120 Uiso 1 1 calc R
H17B H 0.1296 0.3892 0.5282 0.120 Uiso 1 1 calc R
H17C H 0.1505 0.4427 0.6123 0.120 Uiso 1 1 calc R
C18 C -0.00582(15) 0.31113(16) 0.51656(15) 0.0716(7) Uani 1 1 d .
H18A H -0.0406 0.3577 0.4852 0.107 Uiso 1 1 calc R
H18B H -0.0357 0.2701 0.5346 0.107 Uiso 1 1 calc R
H18C H 0.0157 0.2819 0.4810 0.107 Uiso 1 1 calc R
C3 C 0.10095(18) -0.09976(16) 0.97722(16) 0.0716(7) Uani 1 1 d .
H3 H 0.1232 -0.1393 1.0218 0.086 Uiso 1 1 calc R
C14 C 0.33827(16) 0.1975(2) 0.62330(17) 0.0853(9) Uani 1 1 d .
H14A H 0.3921 0.1976 0.6265 0.128 Uiso 1 1 calc R
H14B H 0.3088 0.2453 0.5882 0.128 Uiso 1 1 calc R
H14C H 0.3126 0.1432 0.5991 0.128 Uiso 1 1 calc R
C13 C 0.39047(15) 0.1330(2) 0.7678(2) 0.0922(10) Uani 1 1 d .
H13A H 0.4438 0.1350 0.7695 0.138 Uiso 1 1 calc R
H13B H 0.3660 0.0778 0.7446 0.138 Uiso 1 1 calc R
H13C H 0.3930 0.1393 0.8244 0.138 Uiso 1 1 calc R
C15 C 0.37998(16) 0.2948(2) 0.7514(2) 0.0968(10) Uani 1 1 d .
H15A H 0.4340 0.2961 0.7550 0.145 Uiso 1 1 calc R
H15B H 0.3808 0.3003 0.8073 0.145 Uiso 1 1 calc R
H15C H 0.3500 0.3425 0.7165 0.145 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'
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'
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
N3 Cr1 N3 169.49(9) 2_556 .
N3 Cr1 O1 80.55(6) 2_556 2_556
N3 Cr1 O1 107.03(6) . 2_556
N3 Cr1 O1 107.03(6) 2_556 .
N3 Cr1 O1 80.55(6) . .
O1 Cr1 O1 90.68(8) 2_556 .
N3 Cr1 N1 75.73(7) 2_556 2_556
N3 Cr1 N1 96.91(7) . 2_556
O1 Cr1 N1 156.06(6) 2_556 2_556
O1 Cr1 N1 93.12(6) . 2_556
N3 Cr1 N1 96.91(7) 2_556 .
N3 Cr1 N1 75.73(7) . .
O1 Cr1 N1 93.12(6) 2_556 .
O1 Cr1 N1 156.06(6) . .
N1 Cr1 N1 92.92(9) 2_556 .
C11 O1 Cr1 114.36(11) . .
C1 N1 C5 117.86(19) . .
C1 N1 Cr1 129.22(16) . .
C5 N1 Cr1 112.91(13) . .
N2 N3 C6 120.31(16) . .
N2 N3 Cr1 123.70(13) . .
C6 N3 Cr1 115.85(12) . .
N3 N2 C5 108.66(16) . .
C9 C10 C11 116.43(18) . .
C9 C10 C16 122.83(17) . .
C11 C10 C16 120.71(18) . .
N3 C6 C7 125.90(17) . .
N3 C6 C11 111.09(16) . .
C7 C6 C11 123.01(18) . .
C8 C7 C6 119.20(18) . .
C8 C7 H7 120.4 . .
C6 C7 H7 120.4 . .
O1 C11 C6 117.76(17) . .
O1 C11 C10 124.47(17) . .
C6 C11 C10 117.75(17) . .
N1 C5 N2 118.83(17) . .
N1 C5 C4 121.1(2) . .
N2 C5 C4 120.1(2) . .
C7 C8 C9 117.48(18) . .
C7 C8 C12 122.93(19) . .
C9 C8 C12 119.57(18) . .
C10 C16 C18 110.18(17) . .
C10 C16 C19 109.26(17) . .
C18 C16 C19 109.45(19) . .
C10 C16 C17 111.76(18) . .
C18 C16 C17 108.2(2) . .
C19 C16 C17 107.91(19) . .
C10 C9 C8 125.67(18) . .
C10 C9 H9 117.2 . .
C8 C9 H9 117.2 . .
C1 C2 C3 119.4(2) . .
C1 C2 H2 120.3 . .
C3 C2 H2 120.3 . .
N1 C1 C2 122.8(2) . .
N1 C1 H1 118.6 . .
C2 C1 H1 118.6 . .
C3 C4 C5 119.6(2) . .
C3 C4 H4 120.2 . .
C5 C4 H4 120.2 . .
C14 C12 C13 108.7(2) . .
C14 C12 C8 109.60(18) . .
C13 C12 C8 111.19(18) . .
C14 C12 C15 110.4(2) . .
C13 C12 C15 108.3(2) . .
C8 C12 C15 108.7(2) . .
C16 C19 H19A 109.5 . .
C16 C19 H19B 109.5 . .
H19A C19 H19B 109.5 . .
C16 C19 H19C 109.5 . .
H19A C19 H19C 109.5 . .
H19B C19 H19C 109.5 . .
C16 C17 H17A 109.5 . .
C16 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
C16 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
C16 C18 H18A 109.5 . .
C16 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
C16 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
C4 C3 C2 119.2(2) . .
C4 C3 H3 120.4 . .
C2 C3 H3 120.4 . .
C12 C14 H14A 109.5 . .
C12 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C12 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C12 C13 H13A 109.5 . .
C12 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
C12 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
C12 C15 H15A 109.5 . .
C12 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
C12 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cr1 N3 1.9541(16) 2_556
Cr1 N3 1.9541(16) .
Cr1 O1 1.9659(13) 2_556
Cr1 O1 1.9659(13) .
Cr1 N1 2.0463(17) 2_556
Cr1 N1 2.0463(17) .
O1 C11 1.314(2) .
N1 C1 1.350(3) .
N1 C5 1.365(3) .
N3 N2 1.323(2) .
N3 C6 1.376(2) .
N2 C5 1.373(3) .
C10 C9 1.378(3) .
C10 C11 1.425(3) .
C10 C16 1.529(3) .
C6 C7 1.401(3) .
C6 C11 1.420(3) .
C7 C8 1.366(3) .
C7 H7 0.9300 .
C5 C4 1.397(3) .
C8 C9 1.416(3) .
C8 C12 1.534(3) .
C16 C18 1.533(3) .
C16 C19 1.537(3) .
C16 C17 1.539(3) .
C9 H9 0.9300 .
C2 C1 1.372(3) .
C2 C3 1.374(4) .
C2 H2 0.9300 .
C1 H1 0.9300 .
C4 C3 1.369(3) .
C4 H4 0.9300 .
C12 C14 1.517(3) .
C12 C13 1.531(3) .
C12 C15 1.533(4) .
C19 H19A 0.9600 .
C19 H19B 0.9600 .
C19 H19C 0.9600 .
C17 H17A 0.9600 .
C17 H17B 0.9600 .
C17 H17C 0.9600 .
C18 H18A 0.9600 .
C18 H18B 0.9600 .
C18 H18C 0.9600 .
C3 H3 0.9300 .
C14 H14A 0.9600 .
C14 H14B 0.9600 .
C14 H14C 0.9600 .
C13 H13A 0.9600 .
C13 H13B 0.9600 .
C13 H13C 0.9600 .
C15 H15A 0.9600 .
C15 H15B 0.9600 .
C15 H15C 0.9600 .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139142975
