Molybdenum(vi) tris(amidophenoxide) complexes.
Erickson, Alexander N.; Brown, Seth N.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 15583–15595; doi:10.1039/c8dt03392g

data_7047780
_publ_section_title
;
 Molybdenum(vi) tris(amidophenoxide) complexes.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15583
_journal_page_last               15595
_journal_paper_doi               10.1039/c8dt03392g
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C63 H72 F9 N3 O3 Mo, 2.5(C H Cl3), C2 H3 N'
_chemical_formula_sum            'C67.5 H77.5 Cl7.5 F9 Mo N4 O3'
_chemical_formula_weight         1525.65
_chemical_name_common
;
(^CF3^ap)3Mo . 2.5(CHCl3) . CH3CN
;
_chemical_name_systematic
'Tris-(2-(4-trifluoromethylphenyl)-amido-4,6-di-tert-butylphenoxide)molybdenum(VI) chloroform solvate acetonitrile solvate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-08-15 deposited with the CCDC.
2018-10-16 downloaded from the CCDC.
;
_cell_angle_alpha                94.129(2)
_cell_angle_beta                 100.295(2)
_cell_angle_gamma                117.9600(10)
_cell_formula_units_Z            2
_cell_length_a                   14.1451(7)
_cell_length_b                   15.0385(10)
_cell_length_c                   20.0036(9)
_cell_measurement_reflns_used    9792
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.685
_cell_measurement_theta_min      2.354
_cell_volume                     3638.1(3)
_computing_cell_refinement       'Bruker SAINT (Bruker, 2015)'
_computing_data_collection       'Bruker APEX-3 (Bruker, 2015)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2015)'
_computing_molecular_graphics    'Bruker XP (Bruker, 2015)'
_computing_publication_material  'CIFTAB (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT-2014/2 (Sheldrick, 2015)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker Kappa X8-APEX-II'
_diffrn_measurement_method       'combination of \w and \f-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  0.0693
_diffrn_reflns_av_unetI/netI     0.0587
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            103484
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.365
_diffrn_reflns_theta_min         1.558
_exptl_absorpt_coefficient_mu    0.525
_exptl_absorpt_correction_T_max  0.745700
_exptl_absorpt_correction_T_min  0.671600
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
L. Krause, R. Herbst-Irmer, G. M. Sheldrick & D. Stalke. J. Appl.
Cryst., 2015, 48, 3.
;
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       Rectangular
_exptl_crystal_F_000             1570
_exptl_crystal_recrystallization_method
'Crystals were deposited from a solution of the material dissolvedin chloroform layered with acetonitrile.'
_exptl_crystal_size_max          0.291
_exptl_crystal_size_mid          0.264
_exptl_crystal_size_min          0.180
_exptl_transmission_factor_max   0.745700
_exptl_transmission_factor_min   0.671600
_refine_diff_density_max         1.677
_refine_diff_density_min         -1.580
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     851
_refine_ls_number_reflns         18038
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0909
_refine_ls_R_factor_gt           0.0581
_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/[\s^2^(Fo^2^)+(0.0810P)^2^+6.7220P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1475
_refine_ls_wR_factor_ref         0.1655
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13295
_reflns_number_total             18038
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03392g2.cif
_cod_data_source_block           ANE_230
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Dual' changed to 'dual'
according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/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 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7047780--7047786.cif.
;
_cod_original_formula_sum        'C67.50 H77.50 Cl7.50 F9 Mo N4 O3'
_cod_database_code               7047780
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.862
_shelx_estimated_absorpt_t_max   0.911
_shelx_res_checksum              55805