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_7047782
_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         'C84 H123 Mo N3 O3, C5 H7.50 N2.50, C D Cl3'
_chemical_formula_sum            'C180 H261 Cl6 D2 Mo2 N11 O6'
_chemical_formula_weight         3083.59
_chemical_name_common
;
Mo(^tbu2C6H3^ap)3 . CDCl3 . 2.5(CH3CN)
;
_chemical_name_systematic
'Tris-(2-(3,5-di-tert-butylphenyl)-amido-4,6-di-tert-butylphenoxide)molybdenum(VI) deuterochloroform solvate acetonitrile solvate'
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2018-08-15 deposited with the CCDC.
2018-10-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.1909(16)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.9143(6)
_cell_length_b                   25.9480(12)
_cell_length_c                   24.7282(12)
_cell_measurement_reflns_used    13855
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.342
_cell_measurement_theta_min      2.284
_cell_volume                     8914.2(7)
_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 1.000
_diffrn_measured_fraction_theta_max 0.996
_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  0.0327
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            177017
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.406
_diffrn_reflns_theta_min         1.138
_exptl_absorpt_coefficient_mu    0.285
_exptl_absorpt_correction_T_max  0.74570
_exptl_absorpt_correction_T_min  0.68970
_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    1.149
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       Rectangular
_exptl_crystal_F_000             3308
_exptl_crystal_recrystallization_method
'Crystals were deposited from the reaction mixture in CDCl3which was layered with acetonitrile.'
_exptl_crystal_size_max          0.618
_exptl_crystal_size_mid          0.366
_exptl_crystal_size_min          0.262
_exptl_transmission_factor_max   0.74570
_exptl_transmission_factor_min   0.68970
_refine_diff_density_max         0.902
_refine_diff_density_min         -0.700
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1349
_refine_ls_number_reflns         22286
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0348
_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^)+(0.0471P)^2^+4.2133P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0889
_refine_ls_wR_factor_ref         0.0943
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18567
_reflns_number_total             22286
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03392g2.cif
_cod_data_source_block           final
_cod_depositor_comments
;
The following automatic conversions were performed:

'_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        'C180 H261 D2 Cl6  Mo2 N11 O6'
_cod_database_code               7047782
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.843
_shelx_estimated_absorpt_t_max   0.929
_shelx_res_checksum              25971