#------------------------------------------------------------------------------
#$Date: 2023-05-05 03:26:41 +0300 (Fri, 05 May 2023) $
#$Revision: 283095 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/14/7131418.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_7131418
loop_
_publ_author_name
'Masero, Fabio'
'Mougel, Victor'
_publ_section_title
;
 Molybdenum(IV) β-diketonate complexes as highly active catalysts
 for allylic substitution reactions.
;
_journal_issue                   31
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4636
_journal_page_last               4639
_journal_paper_doi               10.1039/d3cc00572k
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'C10 H14 Cl2 Mo O4'
_chemical_formula_sum            'C10 H14 Cl2 Mo O4'
_chemical_formula_weight         365.05
_chemical_name_systematic        'Molybdenum bis(acetylacetonate) dichloride'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-02-02
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-02-06 deposited with the CCDC.	2023-03-14 downloaded from the CCDC.
;
_cell_angle_alpha                92.355(3)
_cell_angle_beta                 112.501(3)
_cell_angle_gamma                118.207(3)
_cell_formula_units_Z            1
_cell_length_a                   7.2362(5)
_cell_length_b                   7.3583(5)
_cell_length_c                   7.9687(6)
_cell_measurement_reflns_used    5512
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      28.15
_cell_measurement_theta_min      3.26
_cell_volume                     332.36(4)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0198
_diffrn_reflns_av_unetI/netI     0.0174
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            7118
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.462
_diffrn_reflns_theta_min         2.876
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.387
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6848
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0605 before and 0.0470 after correction.
 The Ratio of minimum to maximum transmission is 0.89.

Final HKLF 4 output contains 21648 reflections, Rint = 0.1455
 (6569 with I > 3sig(I), Rint = 0.0793)
;
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.824
_exptl_crystal_description       block
_exptl_crystal_F_000             182
_exptl_crystal_recrystallization_method
'from acetonitrile at -35 degree Celsius'
_exptl_crystal_size_max          0.196
_exptl_crystal_size_mid          0.154
_exptl_crystal_size_min          0.108
_refine_diff_density_max         0.652
_refine_diff_density_min         -0.530
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.195
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     81
_refine_ls_number_reflns         1496
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.195
_refine_ls_R_factor_all          0.0224
_refine_ls_R_factor_gt           0.0220
_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)+0.6511P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0530
_refine_ls_wR_factor_ref         0.0532
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1473
_reflns_number_total             1496
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3cc00572k2.cif
_cod_data_source_block           fma_377_4_0m
_cod_depositor_comments
'Adding full bibliography for 7131417--7131422.cif.'
_cod_database_code               7131418
_shelx_shelxl_version_number     2019/1
_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.
;
_shelx_estimated_absorpt_t_max   0.865
_shelx_estimated_absorpt_t_min   0.773
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3)
2.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C1(H1A,H1B,H1C)
;
_olex2_date_sample_data_collection 2021-03-03
_olex2_date_sample_submission    2021-03-03
_olex2_submission_original_sample_id FMA_377
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.000000 0.500000 0.500000 0.01245(9) Uani 1 2 d S . P . .
Cl1 Cl 0.07275(10) 0.60109(9) 0.81500(8) 0.02117(13) Uani 1 1 d . . . . .
O1 O 0.3348(3) 0.7287(2) 0.5713(2) 0.0172(3) Uani 1 1 d . . . . .
O2 O 0.1245(3) 0.3070(2) 0.5732(2) 0.0170(3) Uani 1 1 d . . . . .
C2 C 0.5266(4) 0.7420(4) 0.6903(3) 0.0159(4) Uani 1 1 d . . . . .
C4 C 0.3355(4) 0.3607(4) 0.6908(3) 0.0163(4) Uani 1 1 d . . . . .
C3 C 0.5315(4) 0.5699(4) 0.7544(3) 0.0181(5) Uani 1 1 d . . . . .
H3 H 0.677916 0.596560 0.847671 0.022 Uiso 1 1 calc R U . . .
C5 C 0.3657(4) 0.1831(4) 0.7535(4) 0.0228(5) Uani 1 1 d . . . . .
H5A H 0.380649 0.188737 0.881408 0.034 Uiso 1 1 calc R U . . .
H5B H 0.507983 0.199487 0.753029 0.034 Uiso 1 1 calc R U . . .
H5C H 0.228107 0.044874 0.667020 0.034 Uiso 1 1 calc R U . . .
C1 C 0.7494(4) 0.9560(4) 0.7548(4) 0.0231(5) Uani 1 1 d . . . . .
H1A H 0.737550 1.026507 0.652874 0.035 Uiso 1 1 calc R U . . .
H1B H 0.882810 0.936411 0.788547 0.035 Uiso 1 1 calc R U . . .
H1C H 0.773795 1.045047 0.865334 0.035 Uiso 1 1 calc R U . . .
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'
Cl Cl 0.1484 0.1585 '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'
O O 0.0106 0.0060 '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
_geom_angle_publ_flag
Cl1 Mo1 Cl1 180.0 . 2_566 ?
O1 Mo1 Cl1 90.60(5) 2_566 . ?
O1 Mo1 Cl1 89.40(5) 2_566 2_566 ?
O1 Mo1 Cl1 90.60(5) . 2_566 ?
O1 Mo1 Cl1 89.40(5) . . ?
O1 Mo1 O1 180.0 2_566 . ?
O1 Mo1 O2 85.88(6) 2_566 2_566 ?
O1 Mo1 O2 85.88(6) . . ?
O1 Mo1 O2 94.12(6) . 2_566 ?
O1 Mo1 O2 94.12(6) 2_566 . ?
O2 Mo1 Cl1 90.77(5) . 2_566 ?
O2 Mo1 Cl1 89.23(5) 2_566 2_566 ?
O2 Mo1 Cl1 90.77(5) 2_566 . ?
O2 Mo1 Cl1 89.23(5) . . ?
O2 Mo1 O2 180.0 . 2_566 ?
C2 O1 Mo1 127.75(14) . . ?
C4 O2 Mo1 127.99(14) . . ?
O1 C2 C3 123.5(2) . . ?
O1 C2 C1 115.9(2) . . ?
C3 C2 C1 120.6(2) . . ?
O2 C4 C3 123.6(2) . . ?
O2 C4 C5 116.4(2) . . ?
C3 C4 C5 120.0(2) . . ?
C2 C3 C4 124.5(2) . . ?
C2 C3 H3 117.7 . . ?
C4 C3 H3 117.7 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 Cl1 2.3656(6) 2_566 ?
Mo1 Cl1 2.3656(6) . ?
Mo1 O1 2.0098(16) 2_566 ?
Mo1 O1 2.0098(16) . ?
Mo1 O2 2.0108(16) 2_566 ?
Mo1 O2 2.0108(16) . ?
O1 C2 1.301(3) . ?
O2 C4 1.292(3) . ?
C2 C3 1.395(3) . ?
C2 C1 1.497(3) . ?
C4 C3 1.400(3) . ?
C4 C5 1.498(3) . ?
C3 H3 0.9500 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
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
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mo1 O1 C2 C3 17.0(3) . . . . ?
Mo1 O1 C2 C1 -164.14(16) . . . . ?
Mo1 O2 C4 C3 -16.4(3) . . . . ?
Mo1 O2 C4 C5 165.81(16) . . . . ?
O1 C2 C3 C4 4.1(4) . . . . ?
O2 C4 C3 C2 -4.4(4) . . . . ?
C5 C4 C3 C2 173.3(2) . . . . ?
C1 C2 C3 C4 -174.8(2) . . . . ?
