Chloro- and Trifluoromethyl-Substituted Flanking-Ring m-Terphenyl Isocyanides: η6-Arene Binding to Zero-Valent Molybdenum Centers and Comparison to Alkyl-Substituted Derivatives
Treffly B. Ditri; Alex E. Carpenter; Donald S. Ripatti; Curtis E. Moore; Arnold L. Rheingold; Joshua S. Figueroa; Inorganic Chemistry 52 (2013) 13216–13229; doi:10.1021/ic402130p

data_4336754
_publ_section_title
;
 Chloro- and Trifluoromethyl-Substituted Flanking-Ring m-Terphenyl
 Isocyanides: \h6-Arene Binding to Zero-Valent Molybdenum Centers and
 Comparison to Alkyl-Substituted Derivatives
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              13216
_journal_page_last               13229
_journal_paper_doi               10.1021/ic402130p
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C79 H35 F36 Mo N3'
_chemical_formula_sum            'C79 H35 F36 Mo N3'
_chemical_formula_weight         1806.04
_chemical_name_common            Mo(C10H8)(CNArDArF2)3
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-08-19
_audit_creation_method
;
  Olex2 1.2-beta
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.8137(3)
_cell_length_b                   22.2232(4)
_cell_length_c                   29.0539(5)
_cell_measurement_reflns_used    6490
_cell_measurement_temperature    100
_cell_measurement_theta_max      50.768
_cell_measurement_theta_min      5.449
_cell_volume                     14084.5(4)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'Bruker APEX2 v2011.4-0 (Bruker, 2011)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
M. C. Burla, R. Caliandro, M. Camalli, B. Carrozzini, G. L. Cascarano, 
L. De Caro, C. Giacovazzo, G. Polidori and R. Spagna, 
SIR2004: an improved tool for crystal structure determination and refinement. 
J. Appl. Cryst. (2005). 38, 381-388.
;
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX CCD'
_diffrn_detector_area_resol_mean 8.0
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.900
_diffrn_measured_fraction_theta_max 0.904
_diffrn_measurement_device       'Fixed Chi Three-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker D8 APEX'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Multilayer Mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0822
_diffrn_reflns_av_unetI/netI     0.0858
_diffrn_reflns_Laue_measured_fraction_full 0.900
_diffrn_reflns_Laue_measured_fraction_max 0.904
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            44903
_diffrn_reflns_point_group_measured_fraction_full 0.900
_diffrn_reflns_point_group_measured_fraction_max 0.904
_diffrn_reflns_theta_full        68.000
_diffrn_reflns_theta_max         67.761
_diffrn_reflns_theta_min         5.407
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_type              'Bruker FR-591'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.850
_exptl_absorpt_correction_T_max  0.7530
_exptl_absorpt_correction_T_min  0.5998
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1270 before and 0.0775 after correction.
The Ratio of minimum to maximum transmission is 0.7965.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            purple
_exptl_crystal_colour_primary    purple
_exptl_crystal_density_diffrn    1.703
_exptl_crystal_description       Block
_exptl_crystal_F_000             7168
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.606
_refine_diff_density_min         -0.739
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1113
_refine_ls_number_reflns         11549
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0864
_refine_ls_R_factor_gt           0.0503
_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^)+(0.0509P)^2^+8.3636P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1117
_refine_ls_wR_factor_ref         0.1270
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7969
_reflns_number_total             11549
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic402130p_si_001_10.cif
_cod_data_source_block           JFigCu94
_cod_database_code               4336754
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 F27-C77
 1.3 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F31) = Uanis(F31A) = Uanis(F1A) = Uanis(F33) = Uanis(F33A) = Uanis(F1B) 
= Uanis(F32) = Uanis(F32A)
Uanis(F6A) = Uanis(F5) = Uanis(F1D) = Uanis(F5A) = Uanis(F4) = Uanis(F1E) 
= Uanis(F4A) = Uanis(F6) = Uanis(F1C)
Uanis(F1I) = Uanis(F26) = Uanis(F1J) = Uanis(F1F) = Uanis(F25) = Uanis(F1G) 
= Uanis(F1H) = Uanis(F27) = Uanis(F1K)
4. others
 1*[Sof(F31)]+1*[Sof(F31A)]+1*[Sof(F1A)]+1*[Sof(F33)]+1*[Sof(F33A)]+1*
 [Sof(F1B)]+1*[Sof(F32)]+1*[Sof(F32A)]=3 with esd of 0.00001
 1*[Sof(F6A)]+1*[Sof(F1C)]+1*[Sof(F6)]+1*[Sof(F4A)]+1*[Sof(F1E)]+1*[Sof(F4)]+1*
 [Sof(F5A)]+1*[Sof(F1D)]+1*[Sof(F5)]=3 with esd of 0.00001
 1*[Sof(F1K)]+1*[Sof(F27)]+1*[Sof(F1H)]+1*[Sof(F1G)]+1*[Sof(F25)]+1*[Sof(F1F)]+
 1*[Sof(F1J)]+1*[Sof(F26)]+1*[Sof(F1I)]=3 with esd of 0.00001
5.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C11(H11), C12(H12), C13(H13),
 C16(H16), C17(H17), C18(H18), C21(H21), C23(H23), C25(H25), C27(H27), C29(H29),
  C30(H30), C40(H40), C39(H39), C38(H38), C47(H47), C45(H45), C43(H43),
 C53(H53), C51(H51), C49(H49), C62(H62), C61(H61), C60(H60), C71(H71), C73(H73),
  C75(H75), C69(H69), C67(H67), C65(H65)
;
_shelx_estimated_absorpt_t_max   0.871
_shelx_estimated_absorpt_t_min   0.600
_shelx_res_checksum              2952
_shelxl_version_number           2013-2