Mixed amidophenolate-catecholates of molybdenum(vi).
Shekar, Sukesh; Brown, Seth N.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 3601–3611; doi:10.1039/c3dt53496k

data_7029149
_publ_section_title
;
 Mixed amidophenolate-catecholates of molybdenum(vi).
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3601
_journal_page_last               3611
_journal_paper_doi               10.1039/c3dt53496k
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C62 H84 Mo N2 O4, 1.5 (C6 H6)'
_chemical_formula_sum            'C71 H93 Mo N2 O4'
_chemical_formula_weight         1134.41
_chemical_name_common            '(tBuClip)Mo(3,5-tBu2Cat) . 1.5 C6H6'
_chemical_name_systematic
; 
 (4,4'-Di-tert-butylbiphenyl-2,2'-bis((2-oxy- 
3,5-di-tert-butylphenyl)amido)-(3,5-di-tert-butylphenylcatecholato)-
molybdenum(VI) sesquibenzene solvate 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 100.0270(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.6883(2)
_cell_length_b                   24.4093(5)
_cell_length_c                   27.7995(6)
_cell_measurement_reflns_used    9972
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.21
_cell_measurement_theta_min      2.42
_cell_volume                     6473.7(2)
_computing_cell_refinement       'APEX2/SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2004; Sheldrick, 2003)'
_computing_molecular_graphics    'XP (Sheldrick, 1998)'
_computing_publication_material  'XCIF (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.949
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device_type  'Bruker APEX-I CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_av_sigmaI/netI    0.0395
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            53342
_diffrn_reflns_theta_full        69.56
_diffrn_reflns_theta_max         69.56
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    2.015
_exptl_absorpt_correction_T_max  0.8088
_exptl_absorpt_correction_T_min  0.3025
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
Blessing, R. H. (1995) Acta Cryst. A51, 33-38. 
  
Sheldrick, G.M. (2008) SADABS v2008/1. Bruker AXS Inc. 
Madison, WI USA. 
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             2428
_exptl_crystal_recrystallization_method
;
Crystals were grown from benzene layered with acetonitrile  
;
_exptl_crystal_size_max          0.78
_exptl_crystal_size_mid          0.76
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.774
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     724
_refine_ls_number_reflns         11671
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0389
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0530P)^2^+4.5950P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0958
_refine_ls_wR_factor_ref         0.1000
_reflns_number_gt                10611
_reflns_number_total             11671
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt53496k.txt
_cod_data_source_block           ss150b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/current/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 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7029149