Bespoke photoreductants: tungsten arylisocyanides.
Sattler, Wesley; Henling, Lawrence M.; Winkler, Jay R.; Gray, Harry B.; Journal of the American Chemical Society 137 (2015) 1198–1205; doi:10.1021/ja510973h

data_4123297
_publ_section_title
;
 Bespoke photoreductants: tungsten arylisocyanides.
;
_journal_issue                   3
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1198
_journal_page_last               1205
_journal_paper_doi               10.1021/ja510973h
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C114 H126 N6 W'
_chemical_formula_sum            'C114 H126 N6 W'
_chemical_formula_weight         1764.05
_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             2014-05-09
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816),
 SHELXL-2014,
 and manual edit
;
_cell_angle_alpha                85.655(6)
_cell_angle_beta                 87.973(6)
_cell_angle_gamma                81.028(5)
_cell_formula_units_Z            2
_cell_length_a                   14.456(3)
_cell_length_b                   18.045(3)
_cell_length_c                   18.803(4)
_cell_measurement_reflns_used    4561
_cell_measurement_temperature    100
_cell_measurement_theta_max      23.145
_cell_measurement_theta_min      2.291
_cell_volume                     4829.6(16)
_computing_cell_refinement       'SAINT V8.34A (Bruker-AXS, 2007)'
_computing_data_collection       'APEX2 2013.6-2 (Bruker-AXS, 2007)'
_computing_data_reduction        'SAINT V8.34A (Bruker-AXS, 2007)'
_computing_molecular_graphics    'DIAMOND 3 (Crystal Impact, 1999)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/2 (Sheldrick, 2014)'
_computing_structure_solution    'XT-2014/1 (Sheldrick, 2012)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.907
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.1448
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.907
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            30730
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.907
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         32.438
_diffrn_reflns_theta_min         1.426
_diffrn_source_current           30
_diffrn_source_power             1.5
_diffrn_source_target            Mo
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.247
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

For component 1:
 wR2(int) was 0.0588 before and 0.0539 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present
;
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_F_000             1852
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.955
_refine_diff_density_min         -1.073
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.350
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1170
_refine_ls_number_reflns         30730
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.350
_refine_ls_R_factor_all          0.1583
_refine_ls_R_factor_gt           0.0776
_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^)+(0.0300P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1152
_refine_ls_wR_factor_ref         0.1283
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17249
_reflns_number_total             30730
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja510973h_si_002.cif
_cod_data_source_block           a13176
_cod_depositor_comments
'Adding full bibliography for 4123295--4123298.cif.'
_cod_original_cell_volume        4829.6(15)
_cod_database_code               4123297
_shelxl_version_number           2014-2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(H14D)=Sof(C153)=Sof(H15J)=Sof(H15K)=Sof(H15L)=1-FVAR(1)
 Sof(H14C)=Sof(C15C)=Sof(H15G)=Sof(H15H)=Sof(H15I)=FVAR(1)
 Sof(C172)=Sof(H172)=Sof(C182)=Sof(H18G)=Sof(H18H)=Sof(H18I)=Sof(C192)=
 Sof(H19G)=Sof(H19H)=Sof(H19I)=1-FVAR(2)
 Sof(C17B)=Sof(H17B)=Sof(C18B)=Sof(H18D)=Sof(H18E)=Sof(H18F)=Sof(C19B)=
 Sof(H19D)=Sof(H19E)=Sof(H19F)=FVAR(2)
 Sof(H14F)=Sof(C154)=Sof(H15P)=Sof(H15Q)=Sof(H15R)=1-FVAR(3)
 Sof(H14E)=Sof(C15D)=Sof(H15M)=Sof(H15N)=Sof(H15O)=FVAR(3)
3.a Ternary CH refined with riding coordinates:
 C14A(H14A), C17A(H17A), C14B(H14B), C17B(H17B), C172(H172), C14C(H14C),
 C14C(H14D), C17C(H17C), C14D(H14E), C14D(H14F), C17D(H17D), C14E(H14G),
 C17E(H17E), C14F(H14H), C17F(H17F)
3.b Aromatic/amide H refined with riding coordinates:
 C4A(H4A), C6A(H6A), C9A(H9A), C10A(H10A), C11A(H11A), C12A(H12A), C13A(H13A),
 C4B(H4B), C6B(H6B), C9B(H9B), C10B(H10B), C11B(H11B), C12B(H12B), C13B(H13B),
 C4C(H4C), C6C(H6C), C9C(H9C), C10C(H10C), C11C(H11C), C12C(H12C), C13C(H13C),
 C4D(H4D), C6D(H6D), C9D(H9D), C10D(H10D), C11D(H11D), C12D(H12D), C13D(H13D),
 C4E(H4E), C6E(H6E), C9E(H9E), C10E(H10E), C11E(H11E), C12E(H12E), C13E(H13E),
 C4F(H4F), C6F(H6F), C9F(H9F), C10F(H10F), C11F(H11F), C12F(H12F), C13F(H13F)
3.c Idealised Me refined as rotating group:
 C15A(H15A,H15B,H15C), C16A(H16A,H16B,H16C), C18A(H18A,H18B,H18C), C19A(H19A,
 H19B,H19C), C15B(H15D,H15E,H15F), C16B(H16D,H16E,H16F), C18B(H18D,H18E,H18F),
 C19B(H19D,H19E,H19F), C182(H18G,H18H,H18I), C192(H19G,H19H,H19I), C15C(H15G,
 H15H,H15I), C153(H15J,H15K,H15L), C16C(H16G,H16H,H16I), C18C(H18J,H18K,H18L),
 C19C(H19J,H19K,H19L), C15D(H15M,H15N,H15O), C154(H15P,H15Q,H15R), C16D(H16J,
 H16K,H16L), C18D(H18M,H18N,H18O), C19D(H19M,H19N,H19O), C15E(H15S,H15T,H15U),
 C16E(H16M,H16N,H16O), C18E(H18P,H18Q,H18R), C19E(H19P,H19Q,H19R), C15F(H15V,
 H15W,H15X), C16F(H16P,H16Q,H16R), C18F(H18S,H18T,H18U), C19F(H19S,H19T,H19U)
;