Pt-Mg, Pt-Ca, and Pt-Zn Lantern Complexes and Metal-Only Donor-Acceptor Interactions.
Baddour, Frederick G.; Hyre, Ariel S.; Guillet, Jesse L.; Pascual, David; Lopez-de-Luzuriaga, José Maria; Alam, Todd M.; Bacon, Jeffrey W.; Doerrer, Linda H.; Inorganic chemistry 56 (2017) 452–469; doi:10.1021/acs.inorgchem.6b02372

data_4344971
_publ_section_title
;
 Pt-Mg, Pt-Ca, and Pt-Zn Lantern Complexes and Metal-Only Donor-Acceptor
 Interactions.
;
_journal_issue                   1
_journal_name_full               'Inorganic chemistry'
_journal_page_first              452
_journal_page_last               469
_journal_paper_doi               10.1021/acs.inorgchem.6b02372
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         '0.5(C56 H44 O10 Pt2 S8 Zn2), 2(C4 H8 O)'
_chemical_formula_sum            'C36 H38 O7 Pt S4 Zn'
_chemical_formula_weight         971.36
_space_group_crystal_system      tetragonal
_space_group_IT_number           120
_space_group_name_Hall           'I -4 -2c'
_space_group_name_H-M_alt        'I -4 c 2'
_symmetry_space_group_name_Hall  'I -4 -2c'
_symmetry_space_group_name_H-M   'I -4 c 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-11-23
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.0932(18)
_cell_length_b                   19.0932(18)
_cell_length_c                   22.727(2)
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      66.826
_cell_measurement_theta_min      4.632
_cell_volume                     8285.1(13)
_computing_cell_refinement       'SAINT (Bruker, 2006)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'SAINT (Bruker, 2006)'
_computing_molecular_graphics    'OLEX2 (Dolmanov, et al. 2009)'
_computing_publication_material  'PublCIF v.1.9.5_c (IUCr)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      299.68
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker Proteum-R'
_diffrn_measurement_method       '\w & \f scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0909
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            43972
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        66.820
_diffrn_reflns_theta_max         66.820
_diffrn_reflns_theta_min         4.632
_diffrn_source                   'rotating anode'
_exptl_absorpt_coefficient_mu    9.169
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.5983
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0984 before and 0.0770 after correction.
The Ratio of minimum to maximum transmission is 0.7948.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_description       block
_exptl_crystal_F_000             3856
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.069
_refine_diff_density_min         -0.895
_refine_diff_density_rms         0.146
_refine_ls_abs_structure_details
;
 Flack x determined using 1594 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.003(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         3642
_refine_ls_number_restraints     156
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0416
_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^)+(0.0776P)^2^+41.4299P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1223
_refine_ls_wR_factor_ref         0.1231
_reflns_Friedel_coverage         0.854
_reflns_Friedel_fraction_full    0.986
_reflns_Friedel_fraction_max     0.986
_reflns_number_gt                3568
_reflns_number_total             3642
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02372_si_002.cif
_cod_data_source_block           baddour18a_1m-last_Compound_4
_cod_depositor_comments
'Adding full bibliography for 4344969--4344972.cif.'
_cod_original_cell_volume        8285.2(18)
_cod_database_code               4344971
_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 O(H) groups
2. Restrained distances
 C1S-C2S
 1.51 with sigma of 0.02
 C4S-C3S
 1.51 with sigma of 0.02
 C2S-C3S
 1.51 with sigma of 0.02
 O1S-C4S
 1.43 with sigma of 0.02
 O1S-C1S
 1.43 with sigma of 0.02
 C10A-C2
 2.47 with sigma of 0.04
 C14A-C2
 2.47 with sigma of 0.04
 C10B-C2
 2.47 with sigma of 0.04
 C14B-C2
 2.47 with sigma of 0.04
 C4A-C1
 2.47 with sigma of 0.04
 C8A-C1
 2.47 with sigma of 0.04
 C8B-C1
 2.47 with sigma of 0.04
 C4B-C1
 2.47 with sigma of 0.04
 C4S-C1S
 2.33 with sigma of 0.04
 C2S-C4S
 2.33 with sigma of 0.04
 C1S-C3S
 2.33 with sigma of 0.04
 O1S-C2S
 2.37 with sigma of 0.04
 O1S-C3S
 2.37 with sigma of 0.04
 C1-C3A \\sim C3B-C1
 with sigma of 0.02
 S3A-C2 \\sim S3B-C2
 with sigma of 0.02
 Pt1-S3A \\sim Pt1-S3B
 with sigma of 0.02
 Pt1-S2A \\sim Pt1-S2B
 with sigma of 0.02
 S2A-C1 \\sim S2B-C1
 with sigma of 0.02
 O3B-C2 \\sim O3A-C2
 with sigma of 0.02
 Zn1-O3B \\sim Zn1-O3A
 with sigma of 0.02
3. Restrained planarity
 O1SB, C1SB, C3SB, C2SB, C4SB
 with sigma of 0.1
 O1S, C4S, C3S, C2S, C1S
 with sigma of 0.1
4. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
Uanis(O2B) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C9A) = Uanis(C9B)
Uanis(C3B) = Uanis(C3A)
Uanis(C4B) = Uanis(C4A)
Uanis(C5B) = Uanis(C5A)
Uanis(C6B) = Uanis(C6A)
Uanis(C7A) = Uanis(C7B)
Uanis(C8A) = Uanis(C8B)
Uanis(S2A) = Uanis(S2B)
Uanis(S3A) = Uanis(S3B)
Uanis(C14A) = Uanis(C14B)
Uanis(C13A) = Uanis(C13B)
Uanis(C12B) = Uanis(C12A)
Uanis(C11B) = Uanis(C11A)
Uanis(C10B) = Uanis(C10A)
Uanis(O3A) = Uanis(O3B)
Uanis(O2A) = Uanis(O2B)
6. Same fragment restrains
{O1S, C4S, C3S, C2S, C1S} sigma for 1-2: 0.02, 1-3: 0.04
as
{O1SB, C1SB, C3SB, C4SB, C2SB}
7. Others
 Sof(O2B)=Sof(O3B)=Sof(S2B)=Sof(S3B)=1-FVAR(1)
 Sof(S3A)=Sof(O3A)=Sof(S2A)=Sof(O2A)=FVAR(1)
 Sof(O1SB)=Sof(C1SB)=Sof(H1SC)=Sof(H1SD)=Sof(C3SB)=Sof(H3SC)=Sof(H3SD)=
 Sof(C4SB)=Sof(H4SC)=Sof(H4SD)=Sof(C2SB)=Sof(H2SC)=Sof(H2SD)=1-FVAR(2)
 Sof(O1S)=Sof(C4S)=Sof(H4SA)=Sof(H4SB)=Sof(C3S)=Sof(H3SA)=Sof(H3SB)=Sof(C2S)=
 Sof(H2SA)=Sof(H2SB)=Sof(C1S)=Sof(H1SA)=Sof(H1SB)=FVAR(2)
 Fixed Sof: C9A(0.5) C10A(0.5) H10A(0.5) C11A(0.5) H11A(0.5) C12A(0.5)
 H12A(0.5) C13A(0.5) H13A(0.5) C14A(0.5) H14A(0.5) C4A(0.5) H4A(0.5) C3A(0.5)
 C8A(0.5) H8A(0.5) C7A(0.5) H7A(0.5) C6A(0.5) H6A(0.5) C5A(0.5) H5A(0.5)
 C9B(0.5) C14B(0.5) H14B(0.5) C13B(0.5) H13B(0.5) C12B(0.5) H12B(0.5) C11B(0.5)
 H11B(0.5) C10B(0.5) H10B(0.5) C3B(0.5) C4B(0.5) H4B(0.5) C5B(0.5) H5B(0.5)
 C6B(0.5) H6B(0.5) C7B(0.5) H7B(0.5) C8B(0.5) H8B(0.5)
 Fixed Uiso: O1S(0.05) C4S(0.05) C3S(0.05) C2S(0.05) C1S(0.05) O1SB(0.05)
 C1SB(0.05) C3SB(0.05) C4SB(0.05) C2SB(0.05)
8.a Secondary CH2 refined with riding coordinates:
 C4S(H4SA,H4SB), C3S(H3SA,H3SB), C2S(H2SA,H2SB), C1S(H1SA,H1SB), C1SB(H1SC,
 H1SD), C3SB(H3SC,H3SD), C4SB(H4SC,H4SD), C2SB(H2SC,H2SD)
8.b Aromatic/amide H refined with riding coordinates:
 C10A(H10A), C11A(H11A), C12A(H12A), C13A(H13A), C14A(H14A), C4A(H4A),
 C8A(H8A), C7A(H7A), C6A(H6A), C5A(H5A), C14B(H14B), C13B(H13B), C12B(H12B),
 C11B(H11B), C10B(H10B), C4B(H4B), C5B(H5B), C6B(H6B), C7B(H7B), C8B(H8B)
8.c Fitted hexagon refined as free rotating group:
 C9A(C10A,C11A,C12A,C13A,C14A), C4A(C3A,C8A,C7A,C6A,C5A), C9B(C14B,C13B,C12B,
 C11B,C10B), C3B(C4B,C5B,C6B,C7B,C8B)
8.d Idealised tetrahedral OH refined as rotating group:
 O1W(H1W)
;
_shelx_res_checksum              25811
_shelx_hkl_checksum              75787
_shelx_fab_checksum              9796
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'