Thiocyanate-Ligated Heterobimetallic {PtM} Lantern Complexes Including a Ferromagnetically Coupled 1D Coordination Polymer.
Guillet, Jesse L.; Bhowmick, Indrani; Shores, Matthew P.; Daley, Christopher J. A.; Gembicky, Milan; Golen, James A.; Rheingold, Arnold L.; Doerrer, Linda H.; Inorganic chemistry 55 (2016) 8099–8109; doi:10.1021/acs.inorgchem.6b01182

data_4348472
_publ_section_title
;
 Thiocyanate-Ligated Heterobimetallic {PtM} Lantern Complexes Including a
 Ferromagnetically Coupled 1D Coordination Polymer.
;
_journal_issue                   16
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8099
_journal_page_last               8109
_journal_paper_doi               10.1021/acs.inorgchem.6b01182
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety
'C9 H12 N Ni O4 Pt S5, C16 H32 Na O8, C3 H6 O'
_chemical_formula_sum            'C28 H50 N Na Ni O13 Pt S5'
_chemical_formula_weight         1045.78
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2016-02-19
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   14.4802(15)
_cell_length_b                   30.199(3)
_cell_length_c                   27.641(3)
_cell_measurement_reflns_used    9861
_cell_measurement_temperature    148(2)
_cell_measurement_theta_max      26.05
_cell_measurement_theta_min      2.71
_cell_volume                     12087(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XM (Sheldrick, 2008)'
_diffrn_ambient_temperature      148.15
_diffrn_measured_fraction_theta_full 0.997
_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  0.0501
_diffrn_reflns_av_unetI/netI     0.0616
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            55845
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.139
_diffrn_reflns_theta_min         1.349
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.263
_exptl_absorpt_correction_T_max  0.0193
_exptl_absorpt_correction_T_min  0.0043
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1106 before and 0.0636 after correction.
The Ratio of minimum to maximum transmission is 0.2228.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.724
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6312
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.157
_refine_diff_density_min         -1.730
_refine_diff_density_rms         0.344
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.504(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1283
_refine_ls_number_reflns         22018
_refine_ls_number_restraints     98
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0489
_refine_ls_shift/su_max          0.074
_refine_ls_shift/su_mean         0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0733P)^2^+7.3236P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1244
_refine_ls_wR_factor_ref         0.1508
_reflns_Friedel_coverage         0.958
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                17409
_reflns_number_total             22018
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01182_si_001.cif
_cod_data_source_block           Compound_5_lhd400ni2
_cod_database_code               4348472
_shelx_estimated_absorpt_t_max   0.567
_shelx_estimated_absorpt_t_min   0.428
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.496(13) 0.504(13)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 O29-C60 = O29-C67 = O30-C61 = O30-C62 = O31-C63 = O31-C64 = O32-C65 = O32-C66
 1.45 with sigma of 0.001
 O29'-C60' = O29'-C67' = O30'-C61' = O30'-C62' = O31'-C63' = O31'-C64'
 1.45 with sigma of 0.001
 O32'-C65' = O32'-C66'
 1.45 with sigma of 0.001
 C60-C61 = C62-C63 = C64-C65 = C66-C67
 1.52 with sigma of 0.001
 C60'-C61' = C62'-C63' = C64'-C65' = C66'-C67'
 1.52 with sigma of 0.001
 O33-C68 = O33-C75 = O34-C69 = O34-C70 = O35-C72 = O35-C71
 1.45 with sigma of 0.001
 O36-C73 = O36-C74
 1.45 with sigma of 0.01
 O33'-C68' = O33'-C75' = O34'-C70' = O34'-C69' = O35'-C72'
 1.45 with sigma of 0.001
 O35'-C72' = O36'-C74' = O36'-C73'
 1.45 with sigma of 0.001
 C68-C69 = C70-C71 = C72-C73 = C74-C75
 1.52 with sigma of 0.001
 C68'-C69' = C70'-C71' = C72'-C73' = C74'-C75'
 1.52 with sigma of 0.001
 Na3-C70'
 2.85 with sigma of 0.01
 C74'-O33' = C70'-O35'
 2 with sigma of 0.01
 C69'-O33'
 2.1 with sigma of 0.02
 C62'-O31'
 2 with sigma of 0.02
 S8-C16 = S9-C14 = S6-C10 = S7-C12
 1.75 with sigma of 0.02
 S8'-C16 = S9'-C14 = S6'-C10 = S7'-C12
 1.75 with sigma of 0.02
 S8-Pt2 = S9-Pt2 = S6-Pt2 = S7-Pt2 = S8'-Pt2 = S9'-Pt2 = S6'-Pt2 = S7'-Pt2
 2.3 with sigma of 0.02
 Ni2-O5 = Ni2-O5' = Ni2-O6 = Ni2-O6' = Ni2-O7 = Ni2-O7' = Ni2-O8 = Ni2-O8'
 2.08 with sigma of 0.02
 O5-C10 = O5'-C10 = O6-C12 = O6'-C12 = O7-C14 = O7'-C14 = O8-C16 = O8'-C16
 1.26 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C46) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(S8) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(O29) = Uanis(O29') = Uanis(O30) = Uanis(O30') = Uanis(O31) = Uanis(O31')
= Uanis(O32) = Uanis(O32')
Uanis(O33) = Uanis(O33') = Uanis(O34) = Uanis(O34') = Uanis(O35) = Uanis(O35')
= Uanis(O36) = Uanis(O36')
Uanis(C60) = Uanis(C60') = Uanis(C61) = Uanis(C61') = Uanis(C62) = Uanis(C62')
= Uanis(C63) = Uanis(C63') = Uanis(C64) = Uanis(C64') = Uanis(C65) =
Uanis(C65') = Uanis(C66) = Uanis(C66')
Uanis(C68) = Uanis(C68') = Uanis(C69) = Uanis(C69') = Uanis(C70) = Uanis(C70')
= Uanis(C71) = Uanis(C71') = Uanis(C72) = Uanis(C72') = Uanis(C73) =
Uanis(C73') = Uanis(C74) = Uanis(C74')
Uanis(C75) = Uanis(C75') = Uanis(C67) = Uanis(C67') = Uanis(C44) = Uanis(C45)
Uanis(C4) = Uanis(C6)
Uanis(C18) = Uanis(C19) = Uanis(C20) = Uanis(C21) = Uanis(C22)
Uanis(C27) = Uanis(C30)
Uanis(C34) = Uanis(C47) = Uanis(C50) = Uanis(C51)
Uanis(C56) = Uanis(C59)
Uanis(O5) = Uanis(O5') = Uanis(O6) = Uanis(O6') = Uanis(O7) = Uanis(O7') =
Uanis(O8) = Uanis(O8')
5. Others
 Sof(O29')=Sof(O30')=Sof(O31')=Sof(O32')=Sof(O33')=Sof(O34')=Sof(O35')=
 Sof(O36')=Sof(C60')=Sof(H60C)=Sof(H60D)=Sof(C61')=Sof(H61C)=Sof(H61D)=
 Sof(C62')=Sof(H62C)=Sof(H62D)=Sof(C63')=Sof(H63C)=Sof(H63D)=Sof(C64')=
 Sof(H64C)=Sof(H64D)=Sof(C65')=Sof(H65C)=Sof(H65D)=Sof(C66')=Sof(H66C)=
 Sof(H66D)=Sof(C67')=Sof(H67C)=Sof(H67D)=Sof(C68')=Sof(H68C)=Sof(H68D)=
 Sof(C69')=Sof(H69C)=Sof(H69D)=Sof(C70')=Sof(H70C)=Sof(H70D)=Sof(C71')=
 Sof(H71C)=Sof(H71D)=Sof(C72')=Sof(H72C)=Sof(H72D)=Sof(C73')=Sof(H73C)=
 Sof(H73D)=Sof(C74')=Sof(H74C)=Sof(H74D)=Sof(C75')=Sof(H75C)=Sof(H75D)=1-FVAR(1)
 Sof(O29)=Sof(O30)=Sof(O31)=Sof(O32)=Sof(O33)=Sof(O34)=Sof(O35)=Sof(O36)=
 Sof(C60)=Sof(H60A)=Sof(H60B)=Sof(C61)=Sof(H61A)=Sof(H61B)=Sof(C62)=Sof(H62A)=
 Sof(H62B)=Sof(C63)=Sof(H63A)=Sof(H63B)=Sof(C64)=Sof(H64A)=Sof(H64B)=Sof(C65)=
 Sof(H65A)=Sof(H65B)=Sof(C66)=Sof(H66A)=Sof(H66B)=Sof(C67)=Sof(H67A)=Sof(H67B)=
 Sof(C68)=Sof(H68A)=Sof(H68B)=Sof(C69)=Sof(H69A)=Sof(H69B)=Sof(C70)=Sof(H70A)=
 Sof(H70B)=Sof(C71)=Sof(H71A)=Sof(H71B)=Sof(C72)=Sof(H72A)=Sof(H72B)=Sof(C73)=
 Sof(H73A)=Sof(H73B)=Sof(C74)=Sof(H74A)=Sof(H74B)=Sof(C75)=Sof(H75A)=Sof(H75B)=
 FVAR(1)
 Sof(S6')=Sof(S7')=Sof(S8')=Sof(S9')=1-FVAR(2)
 Sof(S6)=Sof(S7)=Sof(S8)=Sof(S9)=FVAR(2)
 Sof(O5')=Sof(O6')=Sof(O7')=Sof(O8')=1-FVAR(3)
 Sof(O5)=Sof(O6)=Sof(O7)=Sof(O8)=FVAR(3)
6.a Secondary CH2 refined with riding coordinates:
 C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,
 H48B), C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B),
 C53(H53A,H53B), C54(H54A,H54B), C55(H55A,H55B), C56(H56A,H56B), C57(H57A,H57B),
  C58(H58A,H58B), C59(H59A,H59B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,
 H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B),
 C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B),
  C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B), C60(H60A,
 H60B), C61(H61A,H61B), C62(H62A,H62B), C63(H63A,H63B), C64(H64A,H64B),
 C65(H65A,H65B), C66(H66A,H66B), C67(H67A,H67B), C68(H68A,H68B), C69(H69A,H69B),
  C70(H70A,H70B), C71(H71A,H71B), C72(H72A,H72B), C73(H73A,H73B), C74(H74A,
 H74B), C75(H75A,H75B), C60'(H60C,H60D), C61'(H61C,H61D), C62'(H62C,H62D),
 C63'(H63C,H63D), C64'(H64C,H64D), C65'(H65C,H65D), C66'(H66C,H66D), C67'(H67C,
 H67D), C68'(H68C,H68D), C69'(H69C,H69D), C70'(H70C,H70D), C71'(H71C,H71D),
 C72'(H72C,H72D), C73'(H73C,H73D), C74'(H74C,H74D), C75'(H75C,H75D)
6.b Me refined with riding coordinates:
 C86(H86A,H86B,H86C), C80(H80A,H80B,H80C), C83(H83A,H83B,H83C), C85(H85A,H85B,
 H85C), C88(H88A,H88B,H88C), C82(H82A,H82B,H82C)
6.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C11(H11A,
 H11B,H11C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C),
 C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C26(H26A,H26B,
 H26C)
;
_shelx_res_checksum              94557
_shelx_hkl_checksum              23517
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'