Aminobisphenolate supported tungsten disulphido and dithiolene complexes.
Salojärvi, E; Peuronen, A.; Sillanpää, R; Damlin, P.; Kivelä, H; Lehtonen, A.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 9409–9416; doi:10.1039/c5dt00995b

data_7035051
_publ_section_title
;
 Aminobisphenolate supported tungsten disulphido and dithiolene complexes.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9409
_journal_page_last               9416
_journal_paper_doi               10.1039/c5dt00995b
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         '2(C42 H64 N2 O6 S2 W), 3(C2 H3 N)'
_chemical_formula_sum            'C90 H137 N7 O12 S4 W2'
_chemical_formula_weight         2005.00
_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             2015-01-17
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.12 svn.r3133 for OlexSys, GUI svn.r4987)
;
_audit_update_record
;
2015-03-05 deposited with the CCDC.
2015-04-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.6854(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.18664(9)
_cell_length_b                   34.93266(18)
_cell_length_c                   18.54984(10)
_cell_measurement_reflns_used    22537
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      76.4740
_cell_measurement_theta_min      2.8900
_cell_volume                     9605.34(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3953
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
  1 omega  -44.00   25.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.3676   37.0000 -150.0000 138

  2 omega   57.00   96.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       41.3676 -125.0000 -180.0000 78

  3 omega   41.00  143.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -77.0000 -180.0000 204

  4 omega   86.00  178.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   45.0000  -30.0000 184

  5 omega  100.00  178.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  111.0000  150.0000 156

  6 omega   30.00  109.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000    0.0000 158

  7 omega   29.00  104.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000  120.0000 150

  8 omega -114.00   -6.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.3676  -19.0000   30.0000 216
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0585479000
_diffrn_orient_matrix_UB_12      0.0183266000
_diffrn_orient_matrix_UB_13      0.0388002000
_diffrn_orient_matrix_UB_21      -0.0020796000
_diffrn_orient_matrix_UB_22      -0.0384143000
_diffrn_orient_matrix_UB_23      0.0400511000
_diffrn_orient_matrix_UB_31      0.0858204000
_diffrn_orient_matrix_UB_32      0.0115526000
_diffrn_orient_matrix_UB_33      0.0715227000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0186
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_laue_measured_fraction_full 0.996
_diffrn_reflns_laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            34863
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.998
_diffrn_reflns_theta_min         2.893
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.644
_exptl_absorpt_correction_T_max  0.628
_exptl_absorpt_correction_T_min  0.245
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_description       block
_exptl_crystal_F_000             4136
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.2318
_exptl_crystal_size_mid          0.1728
_exptl_crystal_size_min          0.1136
_refine_diff_density_max         0.605
_refine_diff_density_min         -0.845
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1133
_refine_ls_number_reflns         17789
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0254
_refine_ls_R_factor_gt           0.0233
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0257P)^2^+5.6122P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0552
_refine_ls_wR_factor_ref         0.0563
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16708
_reflns_number_total             17789
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00995b1.cif
_cod_data_source_block           4dt
_cod_depositor_comments
'Adding full bibliography for 7035048--7035052.cif.'
_cod_original_cell_volume        9605.33(10)
_cod_database_code               7035051
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C90 H73 N7 O8 S4 W2'
_reflns_odcompleteness_completeness 99.59
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Uiso/Uaniso restraints and constraints
C73A \\sim C73B: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.002
C72A \\sim C72B: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.002
C81 \\sim C82 \\sim C83 \\sim C84: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.002
C74A \\sim C74B: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.002
3. Others
 Sof(C34B)=Sof(H34D)=Sof(H34E)=Sof(H34F)=Sof(C35B)=Sof(H35D)=Sof(H35E)=
 Sof(H35F)=Sof(C36B)=Sof(H36D)=Sof(H36E)=Sof(H36F)=1-FVAR(1)
 Sof(C34A)=Sof(H34A)=Sof(H34B)=Sof(H34C)=Sof(C35A)=Sof(H35A)=Sof(H35B)=
 Sof(H35C)=Sof(C36A)=Sof(H36A)=Sof(H36B)=Sof(H36C)=FVAR(1)
 Sof(C72B)=Sof(H72D)=Sof(H72E)=Sof(H72F)=Sof(C73B)=Sof(H73D)=Sof(H73E)=
 Sof(H73F)=Sof(C74B)=Sof(H74D)=Sof(H74E)=Sof(H74F)=1-FVAR(2)
 Sof(C72A)=Sof(H72A)=Sof(H72B)=Sof(H72C)=Sof(C73A)=Sof(H73A)=Sof(H73B)=
 Sof(H73C)=Sof(C74A)=Sof(H74A)=Sof(H74B)=Sof(H74C)=FVAR(2)
4.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C27B(H27A,H27B), C55(H55A,H55B), C57(H57A,H57B), C58(H58A,H58B),
 C60(H60A,H60B), C7(H7A,H7B), C9(H9A,H9B), C10(H10A,H10B), C12(H12A,H12B),
 C38(H38A,H38B), C47(H47A,H47B)
4.b Aromatic/amide H refined with riding coordinates:
 C51(H51), C53(H53), C62(H62), C64(H64), C3(H3), C5(H5), C14(H14), C16(H16)
4.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C28B(H28A,H28B,H28C), C68(H68A,H68B,H68C), C69(H69A,H69B,
 H69C), C70(H70A,H70B,H70C), C72A(H72A,H72B,H72C), C72B(H72D,H72E,H72F),
 C73A(H73A,H73B,H73C), C73B(H73D,H73E,H73F), C74A(H74A,H74B,H74C), C74B(H74D,
 H74E,H74F), C75(H75A,H75B,H75C), C76(H76A,H76B,H76C), C78(H78A,H78B,H78C),
 C79(H79A,H79B,H79C), C80(H80A,H80B,H80C), C82(H82A,H82B,H82C), C83(H83A,H83B,
 H83C), C84(H84A,H84B,H84C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,
 H22B,H22C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C),
 C27(H27C,H27D,H27E), C28(H28D,H28E,H28F), C30(H30A,H30B,H30C), C31(H31A,H31B,
 H31C), C32(H32A,H32B,H32C), C34A(H34A,H34B,H34C), C34B(H34D,H34E,H34F),
 C35A(H35A,H35B,H35C), C35B(H35D,H35E,H35F), C36A(H36A,H36B,H36C), C36B(H36D,
 H36E,H36F), C37(H37A,H37B,H37C), C48(H48A,H48B,H48C), C90(H90A,H90B,H90C),
 C93(H93A,H93B,H93C), C87(H87A,H87B,H87C)
;
_olex2_submission_special_instructions 'No special instructions were received'