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_4336760
_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         'C72 H27 F36 Mo N3 O3'
_chemical_formula_sum            'C72 H27 F36 Mo N3 O3'
_chemical_formula_weight         1761.91
_chemical_name_common            mer-Mo(CO)3(CNArDArF2)3
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 100.681(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.1623(18)
_cell_length_b                   16.5584(11)
_cell_length_c                   31.990(2)
_cell_measurement_reflns_used    9960
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.346
_cell_measurement_theta_min      2.591
_cell_volume                     13618.2(16)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_collection       'Bruker APEX2 v2013-2.0 (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_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-II CCD'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker X8 APEX II'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_unetI/netI     0.0445
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            48889
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.490
_diffrn_reflns_theta_min         1.296
_diffrn_source                   'sealed tube'
_diffrn_source_type              fine-focus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.344
_exptl_absorpt_correction_T_max  0.2590
_exptl_absorpt_correction_T_min  0.2196
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0836 before and 0.0468 after correction.
The Ratio of minimum to maximum transmission is 0.8479.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.719
_exptl_crystal_description       Block
_exptl_crystal_F_000             6960
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.594
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1052
_refine_ls_number_reflns         12563
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0454
_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^)+(0.0931P)^2^+12.1605P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1228
_refine_ls_wR_factor_ref         0.1521
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9677
_reflns_number_total             12563
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic402130p_si_001_16.cif
_cod_data_source_block           JFig833
_cod_original_cell_volume        13617.9(16)
_cod_database_code               4336760
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(F32A) = Uanis(F32)
Uanis(F33A) = Uanis(F33)
Uanis(F18) = Uanis(F18A)
Uanis(F1D) = Uanis(F17) = Uanis(F1C) = Uanis(F18A) = Uanis(F18) = Uanis(F1A) 
= Uanis(F1B) = Uanis(F16)
Uanis(F1F) = Uanis(F9) = Uanis(F9A) = Uanis(F1G) = Uanis(F7) = Uanis(F1E) 
= Uanis(F7A) = Uanis(F8) = Uanis(F8A) = Uanis(C26)
Uanis(F35A) = Uanis(F35) = Uanis(F1I) = Uanis(F36A) = Uanis(F36) = Uanis(F1H) 
= Uanis(F34A) = Uanis(F34) = Uanis(F1J)
3. others
 Sof(F32A)=Sof(F33A)=1-FVAR(1)
 Sof(F32)=Sof(F33)=FVAR(1)
 Fixed Sof: F1A(0.36059) F1B(0.17981) F1C(0.17903) F1D(0.08332) F1E(0.20038)
 F1F(0.19553) F1G(0.13643) F1H(0.1945) F1I(0.17125) F1J(0.10608) F7(0.46328)
 F7A(0.63825) F8(0.23241) F8A(0.2231) F9(0.33223) F9A(0.5784) F16(0.71759)
 F17(0.73519) F18(0.45397) F18A(0.2905) F34(0.45469) F34A(0.4489) F35(0.27763)
 F35A(0.62009) F36(0.30799) F36A(0.41889)
4.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C11(H11), C14(H14), C16(H16), C18(H18), C20(H20), C22(H22),
 C24(H24), C31(H31), C32(H32), C33(H33), C36(H36), C38(H38), C40(H40), C42(H42),
  C44(H44), C46(H46), C53(H53), C54(H54), C55(H55), C58(H58), C60(H60),
 C62(H62), C64(H64), C66(H66), C68(H68)
;
_shelx_estimated_absorpt_t_max   0.973
_shelx_estimated_absorpt_t_min   0.950
_shelx_res_checksum              43511
_shelxl_version_number           2013-2