N-Heterocyclic Carbene Adducts of Molybdenum Tetracarboxylate Complexes
Robinson, Thomas P.; Johnson, Andrew L.; Raithby, Paul R.; Kociok-Kohn, Gabriele; Organometallics 35 (2016) 2494–; doi:10.1021/acs.organomet.6b00386

data_4086604
_publ_section_title
;
 N-Heterocyclic Carbene Adducts of Molybdenum Tetracarboxylate Complexes
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              2494
_journal_paper_doi               10.1021/acs.organomet.6b00386
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C26 H46 Cl2 Mo2 N4 O4, 2(C7 H8)'
_chemical_formula_sum            'C40 H62 Cl2 Mo2 N4 O4'
_chemical_formula_weight         925.71
_chemical_name_systematic
;
 ?
;
_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     direct
_audit_creation_date             2016-07-01
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                102.5570(10)
_cell_angle_beta                 106.2100(10)
_cell_angle_gamma                93.4270(10)
_cell_formula_units_Z            1
_cell_length_a                   9.8940(2)
_cell_length_b                   11.8630(2)
_cell_length_c                   12.7570(3)
_cell_measurement_reflns_used    8488
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      2.5
_cell_volume                     1391.76(5)
_computing_cell_refinement       "'HKL Scalepack (Otwinowski"
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
;
 DENZO-SCALEPACK Z. Otwinowski and W. Minor, " 
 Processing of X-ray Diffraction Data Collected in Oscillation Mode ", 
 Methods in Enzymology, Volume 276: Macromolecular Crystallography, 
 part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press.
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Enraf Nonius Kappa Diffractometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8488
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.687
_diffrn_reflns_theta_min         3.544
_diffrn_source                   ' fine focus sealed tube'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.579
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Sortav
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.104
_exptl_crystal_description       block
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   1.00
_exptl_transmission_factor_min   0.85
_platon_squeeze_details
;
Additional solvent that could not be modelled was
removed using PLATON SQUEEZE
;
_refine_diff_density_max         1.831
_refine_diff_density_min         -0.750
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         8488
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0761P)^2^+0.7224P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1174
_refine_ls_wR_factor_ref         0.1212
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7710
_reflns_number_total             8488
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00386_si_002.cif
_cod_data_source_block           '[HL4][Mo2(OPiv)5]_(4)'
_cod_depositor_comments
'Adding full bibliography for 4086597--4086604.cif.'
_cod_database_code               4086604
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.944
_shelx_estimated_absorpt_t_min   0.893
_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. Others
Fixed Sof: C1S(0.65) C2S(0.65) H2S(0.65) C3S(0.65) H3S(0.65) C4S(0.65)
H4S(0.65) C5S(0.65) H5S(0.65) C6S(0.65) H6S(0.65) C7S(0.65) H7SA(0.65)
H7SB(0.65) H7SC(0.65) C11S(0.35) C12S(0.35) H12S(0.35) C13S(0.35) H13S(0.35)
C14S(0.35) H14S(0.35) C15S(0.35) H15S(0.35) C16S(0.35) H16S(0.35) C17S(0.35)
H17A(0.35) H17B(0.35) H17C(0.35)
3.a Ternary CH refined with riding coordinates:
C11(H11), C21(H21)
3.b Me refined with riding coordinates:
C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C22(H22A,H22B,H22C), C23(H23A,H23B,
H23C)
3.c Aromatic/amide H refined with riding coordinates:
C2S(H2S), C3S(H3S), C4S(H4S), C5S(H5S), C6S(H6S), C12S(H12S), C13S(H13S),
C14S(H14S), C15S(H15S), C16S(H16S)
3.d Fitted hexagon refined as free rotating group:
C1S(C2S,C3S,C4S,C5S,C6S)
3.e Idealised Me refined as rotating group:
C32(H32A,H32B,H32C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C7S(H7SA,H7SB,H7SC),
C17S(H17A,H17B,H17C)
;
_olex2_exptl_crystal_mounting_method 'Fomblin oil on a glass fibre'
_olex2_submission_original_sample_id k09alj29
_olex2_submission_special_instructions 'No special instructions were received'