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_4123295
_publ_section_title
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 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         'C132 H162 N6 O18 W'
_chemical_formula_sum            'C132 H162 N6 O18 W'
_chemical_formula_weight         2304.52
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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
_audit_creation_date             2014-05-20
_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                90
_cell_angle_beta                 91.886(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.6451(10)
_cell_length_b                   20.7417(11)
_cell_length_c                   21.9870(16)
_cell_measurement_reflns_used    9949
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.08
_cell_measurement_theta_min      2.34
_cell_volume                     6219.4(7)
_computing_cell_refinement       'SAINT V8.34A (Bruker-AXS, 2007)'
_computing_data_collection       'APEX2 2014.1-1 (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 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2268
_diffrn_reflns_av_unetI/netI     0.2103
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            122616
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         33.971
_diffrn_reflns_theta_min         1.350
_diffrn_source_current           30
_diffrn_source_power             1.5
_diffrn_source_target            Mo
_diffrn_source_voltage           50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.994
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8699
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0739 before and 0.0674 after correction.
The Ratio of minimum to maximum transmission is 0.8699.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_F_000             2428
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.974
_refine_diff_density_min         -1.061
_refine_diff_density_rms         0.136
_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     766
_refine_ls_number_reflns         25166
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1964
_refine_ls_R_factor_gt           0.0747
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0500P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1263
_refine_ls_wR_factor_ref         0.1597
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11195
_reflns_number_total             25166
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja510973h_si_004.cif
_cod_data_source_block           a13160
_cod_depositor_comments
'Adding full bibliography for 4123295--4123298.cif.'
_cod_database_code               4123295
_shelxl_version_number           2014-2
_shelx_estimated_absorpt_t_max   0.916
_shelx_estimated_absorpt_t_min   0.710
_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(C44B)=Sof(H44B)=Sof(C45B)=Sof(H45A)=Sof(H45B)=Sof(H45C)=Sof(C46B)=
 Sof(H46A)=Sof(H46B)=Sof(H46C)=1-FVAR(1)
 Sof(C14B)=Sof(H14B)=Sof(C15B)=Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(C16B)=
 Sof(H16D)=Sof(H16E)=Sof(H16F)=FVAR(1)
 Sof(C48B)=Sof(H48A)=Sof(H48B)=Sof(H48C)=Sof(H17C)=1-FVAR(2)
 Sof(H17B)=Sof(C18B)=Sof(H18D)=Sof(H18E)=Sof(H18F)=FVAR(2)
3.a Ternary CH refined with riding coordinates:
 C14A(H14A), C17A(H17A), C14B(H14B), C44B(H44B), C17B(H17C), C17B(H17B),
 C14C(H14C), C17C(H17D)
3.b Aromatic/amide H refined with riding coordinates:
 C4A(H4A), C6A(H6A), C9A(H9A), C13A(H13A), C4B(H4B), C6B(H6B), C9B(H9B),
 C13B(H13B), C4C(H4C), C6C(H6C), C9C(H9C), C13C(H13C)
3.c Idealised Me refined as rotating group:
 C15A(H15A,H15B,H15C), C16A(H16A,H16B,H16C), C18A(H18A,H18B,H18C), C19A(H19A,
 H19B,H19C), C20A(H20A,H20B,H20C), C21A(H21A,H21B,H21C), C22A(H22A,H22B,H22C),
 C15B(H15D,H15E,H15F), C16B(H16D,H16E,H16F), C45B(H45A,H45B,H45C), C46B(H46A,
 H46B,H46C), C48B(H48A,H48B,H48C), C18B(H18D,H18E,H18F), C19B(H19D,H19E,H19F),
 C20B(H20D,H20E,H20F), C21B(H21D,H21E,H21F), C22B(H22D,H22E,H22F), C15C(H15G,
 H15H,H15I), C16C(H16G,H16H,H16I), C18C(H18G,H18H,H18I), C19C(H19G,H19H,H19I),
 C20C(H20G,H20H,H20I), C21C(H21G,H21H,H21I), C22C(H22G,H22H,H22I)
;