Activation of CS2 by a "masked" terminal nickel sulfide.
Hartmann, Nathaniel J.; Wu, Guang; Hayton, Trevor W.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 14508–14510; doi:10.1039/c6dt00885b

data_7039098
_publ_section_title
;
 Activation of CS2 by a &quot;masked&quot; terminal nickel sulfide.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14508
_journal_page_last               14510
_journal_paper_doi               10.1039/c6dt00885b
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C36 H53 N2 Ni S3, C12 H24 K O6, C7 H8'
_chemical_formula_sum            'C55 H85 K N2 Ni O6 S3'
_chemical_formula_weight         1064.23
_chemical_name_systematic
'(trithiocarbonate-\k2-S,S)- (N,N'-bis(2,6-di-isopropylphenyl)-2,2,6,6-tetramethylheptane-3,5-di-iminato)-(1,4,7,10,13,16-hexaoxacyclooctadecane)-nickel(II)-potassium'
_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
_audit_creation_date             2016-03-21
_audit_creation_method
;
Olex2 1.2-dev
(compiled 2016.03.03 svn.r3266 for OlexSys, GUI svn.r3563)
;
_audit_update_record
;
2016-04-07 deposited with the CCDC.
2016-04-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.149(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.647(2)
_cell_length_b                   17.840(2)
_cell_length_c                   18.241(2)
_cell_measurement_reflns_used    181
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24
_cell_measurement_theta_min      21.5
_cell_volume                     5709.6(11)
_computing_data_collection       'BRUKER APEXII v2014.11-0'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.97
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Kappa Apex II'
_diffrn_measurement_method       'Omega scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1186
_diffrn_reflns_av_unetI/netI     0.1234
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            35379
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.408
_diffrn_reflns_theta_min         1.161
_exptl_absorpt_coefficient_mu    0.570
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6471
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2288
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.630
_refine_diff_density_min         -0.485
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     791
_refine_ls_number_reflns         11684
_refine_ls_number_restraints     558
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.1378
_refine_ls_R_factor_gt           0.0629
_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^)+(0.0441P)^2^+2.5896P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1118
_refine_ls_wR_factor_ref         0.1359
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6494
_reflns_number_total             11684
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00885b2.cif
_cod_data_source_block           nh_3_138_0m
_cod_depositor_comments
'Adding full bibliography for 7039098--7039099.cif.'
_cod_original_cell_volume        5709.8(12)
_cod_database_code               7039098
_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. Restrained distances
 O6B-C12B \\sim O6B-C11B \\sim O5-C10 \\sim O5-C9 \\sim O5B-C10B \\sim O5B-C9B
\\sim O3-C8 \\sim O3-C7 ~
 O3B-C8B \\sim O3B-C7B \\sim O2-C6 \\sim O2-C5 \\sim O2B-C6B \\sim O2B-C5B
\\sim O1-C4 \\sim O1-C3 \\sim O1B-
 C4B \\sim O1B-C3B \\sim O4-C2 \\sim O4-C13 \\sim O4B-C2B \\sim O4B-C13B \\sim
O6-C12 \\sim O6-C11
 with sigma of 0.02
 C11-C10 \\sim C11B-C10B \\sim C9-C8 \\sim C9B-C8B \\sim C7-C6 \\sim C7B-C6B
\\sim C5-C4 \\sim C5B-C4B ~
 C3-C2 \\sim C3B-C2B \\sim C13-C12 \\sim C13B-C12B
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 O5, C2, C3, O4, O1, C13, C4, C12, O2, O3, O6, C5, C6, C7, C8, C9, C10, C11
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O5B, C2B, C3B, O4B, O1B, C13B, C4B, C12B, O6B, O2B, O3B, C5B, C11B, C9B, C10B,
  C6B, C7B, C8B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(C2B)=Sof(H2BA)=Sof(H2BB)=Sof(C3B)=Sof(H3BA)=Sof(H3BB)=Sof(C4B)=Sof(H4BA)=
 Sof(H4BB)=Sof(C5B)=Sof(H5BA)=Sof(H5BB)=Sof(C6B)=Sof(H6BA)=Sof(H6BB)=Sof(C7B)=
 Sof(H7BA)=Sof(H7BB)=Sof(C8B)=Sof(H8BA)=Sof(H8BB)=Sof(C9B)=Sof(H9BA)=Sof(H9BB)=
 Sof(C10B)=Sof(H10C)=Sof(H10D)=Sof(C11B)=Sof(H11I)=Sof(H11J)=Sof(C12B)=
 Sof(H12C)=Sof(H12D)=Sof(C13B)=Sof(H13C)=Sof(H13D)=Sof(O1B)=Sof(O2B)=Sof(O3B)=
 Sof(O4B)=Sof(O5B)=Sof(O6B)=1-FVAR(1)
 Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C4)=Sof(H4A)=Sof(H4B)=
 Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(C7)=Sof(H7A)=Sof(H7B)=
 Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(C10)=Sof(H10A)=
 Sof(H10B)=Sof(C11)=Sof(H11G)=Sof(H11H)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(C13)=
 Sof(H13A)=Sof(H13B)=Sof(O1)=Sof(O2)=Sof(O3)=Sof(O4)=Sof(O5)=Sof(O6)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C19(H19), C28(H28), C33(H33), C119(H119)
5.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B),
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11G,H11H), C12(H12A,H12B),
 C13(H13A,H13B), C2B(H2BA,H2BB), C3B(H3BA,H3BB), C4B(H4BA,H4BB), C5B(H5BA,H5BB),
  C6B(H6BA,H6BB), C7B(H7BA,H7BB), C8B(H8BA,H8BB), C9B(H9BA,H9BB), C10B(H10C,
 H10D), C11B(H11I,H11J), C12B(H12C,H12D), C13B(H13C,H13D)
5.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C27(H27), C29(H29), C35(H35), C113(H113), C210(H210), C211(H211),
 C213(H213), C217(H217), C219(H219), C310(H310), C318(H318)
5.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C24(H24A,H24B,H24C), C31(H31A,H31B,H31C), C32(H32A,H32B,
 H32C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C110(H11A,H11B,H11C),
 C112(H11D,H11E,H11F), C212(H21A,H21B,H21C), C214(H21D,H21E,H21F), C218(H21G,
 H21H,H21I), C220(H22A,H22B,H22C), C312(H31J,H31K,H31L), C313(H31D,H31E,H31F),
 C319(H31G,H31H,H31I)
;
_shelx_res_checksum              30206
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'