cis-Dipyridyl Porphyrin-Based Multicomponent Organoplatinum(II) Bismetallacycles for Photocatalytic Oxidation
Cheng, Ying; Zhang, Zeyuan; Duan, Xianglong; Zhang, Mingming; Dalton Transactions  (2022) –; doi:10.1039/D2DT02197H

data_7711470
_publ_section_title
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 cis-Dipyridyl Porphyrin-Based Multicomponent Organoplatinum(II)
 Bismetallacycles for Photocatalytic Oxidation
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_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02197H
_journal_year                    2022
_chemical_formula_moiety         'C148 H178 N12 O8 P8 Pt4, 16[C2H3N], 5[C6H14O]'
_chemical_formula_sum            'C210 H296 N28 O13 P8 Pt4'
_chemical_formula_weight         4448.85
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2022-10-06
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
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2022-10-09 deposited with the CCDC.	2022-10-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.216(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.577(4)
_cell_length_b                   32.060(4)
_cell_length_c                   39.781(4)
_cell_measurement_reflns_used    9873
_cell_measurement_temperature    193.0
_cell_measurement_theta_max      51.18
_cell_measurement_theta_min      2.40
_cell_volume                     40209(8)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/1 (Sheldrick, 2015)'
_diffrn_ambient_temperature      193.0
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.997
_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_unetI/netI     0.0601
_diffrn_reflns_Laue_measured_fraction_full 0.940
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            34193
_diffrn_reflns_point_group_measured_fraction_full 0.940
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.713
_diffrn_reflns_theta_min         0.906
_exptl_absorpt_coefficient_mu    2.906
_exptl_absorpt_correction_T_max  0.7506
_exptl_absorpt_correction_T_min  0.4875
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1304 before and 0.0920 after correction.
The Ratio of minimum to maximum transmission is 0.6495.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_description       block
_exptl_crystal_F_000             18304
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.344
_refine_diff_density_min         -2.343
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.188
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1520
_refine_ls_number_reflns         34193
_refine_ls_number_restraints     1832
_refine_ls_restrained_S_all      1.193
_refine_ls_R_factor_all          0.1491
_refine_ls_R_factor_gt           0.1157
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1200P)^2^+300.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3025
_refine_ls_wR_factor_ref         0.3238
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20690
_reflns_number_total             34193
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02197h2.cif
_cod_data_source_block           539
_cod_original_cell_volume        40210(7)
_cod_database_code               7711470
_shelxl_version_number           2014-1
_shelx_estimated_absorpt_t_max   0.760
_shelx_estimated_absorpt_t_min   0.704
_olex2_refinement_description
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1. Twinned data refinement
 Scales: 0.54(3)
 0.46(3)
2. 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
3. Restrained distances
 C358-C167
 1.52 with sigma of 0.02
 C239-C237
 1.45 with sigma of 0.02
 C147-C141
 1.45 with sigma of 0.02
 C337-C129
 1.45 with sigma of 0.02
 C352-C310
 1.45 with sigma of 0.02
 C41-C261
 1.45 with sigma of 0.02
 C89-C177
 1.45 with sigma of 0.02
 C37-C331
 1.45 with sigma of 0.02
 C49-C270
 1.5 with sigma of 0.02
 C144-C201
 1.5 with sigma of 0.02
 H17B-H81C
 2.1 with sigma of 0.02
 H34D-H89B
 2.1 with sigma of 0.02
 C261-C41
 1.48 with sigma of 0.02
 P94-C261
 1.93 with sigma of 0.02
 C41-C141
 4.1 with sigma of 0.02
 H25C-H41A
 2.1 with sigma of 0.02
 H13A-H41B
 2.1 with sigma of 0.02
 H25B-H41A
 2.1 with sigma of 0.02
 C174-C146
 1.47 with sigma of 0.01
 P94-C41
 3.208 with sigma of 0.04
 C9-C198 \\sim C308-C222 \\sim C84-C16 \\sim C8-C238 \\sim C46-C38 \\sim
C160-C154 \\sim C49-C270 ~
 C185-C180
 with sigma of 0.02
 C270-C132 \\sim C348-C270 \\sim C308-C194 \\sim C346-C308 \\sim C226-C198
\\sim C198-C168 \\sim C180-
 C121 \\sim C280-C180 \\sim C8-C224 \\sim C8-C108 \\sim C84-C70 \\sim C84-C26
\\sim C160-C14 \\sim C160-
 C156 \\sim C38-C164 \\sim C38-C146
 with sigma of 0.02
 C324-C274 \\sim C274-C194 \\sim C348-C324 \\sim C252-C132 \\sim C252-C248
\\sim C280-C248 \\sim C296-
 C121 \\sim C3-C296 \\sim C3-C168 \\sim C346-C128 \\sim C136-C128 \\sim
C226-C136 \\sim C250-C224 ~
 C250-C174 \\sim C174-C146 \\sim C290-C164 \\sim C290-C216 \\sim C216-C156
\\sim C192-C14 \\sim C192-C1
 \\sim C26-C1 \\sim C70-C178 \\sim C300-C178 \\sim C300-C108
 with sigma of 0.02
 C287-C269 \\sim C69-C255 \\sim C41-C261 \\sim C35-C135 \\sim C239-C237 \\sim
C147-C141 \\sim C337-
 C129 \\sim C345-C301 \\sim C21-C159 \\sim C89-C177 \\sim C81-C77 \\sim
C37-C331 \\sim C361-C342 \\sim C27-
 C123 \\sim C282-C264 \\sim C95-C212 \\sim C328-C243 \\sim C352-C310 \\sim
C330-C241 \\sim C349-C173 ~
 C358-C167 \\sim C79-C175 \\sim C356-C219 \\sim C231-C199
 with sigma of 0.02
4. Rigid bond restraints
 C261, C41
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C141, C147
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within -2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within -2A
6.a Riding coordinates:
 C231(H23A,H23B,H23C), C358(H35F,H35G,H35H), C147(H14C,H14D,H14E), C237(H23F,
 H23G,H23H), C159(H15A,H15B,H15C), C337(H33F,H33G,H33H)
6.b Secondary CH2 refined with riding coordinates:
 C212(H21A,H21B), C264(H26A,H26B), C310(H31A,H31B), C328(H32A,H32B), C330(H33A,
 H33B), C342(H34A,H34B), C356(H35A,H35B), C27(H27A,H27B), C199(H19A,H19B),
 C135(H13A,H13B), C141(H14A,H14B), C261(H26C,H26D), C129(H12A,H12B), C69(H69A,
 H69B), C287(H28D,H28E), C239(H23D,H23E), C77(H77A,H77B), C37(H37A,H37B),
 C21(H21F,H21G), C345(H34C,H34D), C177(H17A,H17B), C167(H16A,H16B), C173(H17C,
 H17D), C79(H79A,H79B)
6.c Aromatic/amide H refined with riding coordinates:
 C240(H240), C104(H104), C204(H204), C210(H210), C1(H1), C234(H234),
 C130(H130), C286(H286), C334(H334), C120(H120), C20(H20), C48(H48), C116(H116),
  C122(H122), C268(H268), C306(H306), C318(H318), C228(H228), C74(H74),
 C78(H78), C200(H200), C216(H216), C174(H174), C124(H124), C56(H56), C202(H202),
  C192(H192), C136(H136), C128(H128), C178(H178), C152(H152), C162(H162),
 C184(H184), C260(H260), C254(H254), C290(H290), C252(H252), C324(H324),
 C300(H300), C274(H274), C250(H250), C248(H248), C296(H296), C189(H189),
 C217(H217), C205(H205), C109(H109), C53(H53), C3(H3), C227(H227), C7(H7),
 C51(H51), C115(H115), C207(H207), C245(H245), C63(H63), C265(H265), C259(H259)
6.d Fitted hexagon refined as free rotating group:
 N86(C240,C104,C16,C204,C210), N36(C234,C130,C238,C286,C334), C46(C120,C20,C48,
 C116,C122), N76(C268,C306,C222,C318,C228), C148(C74,C232,C78,C230,C200),
 C220(C124,C144,C56,C42,C202), C154(C152,C162,C184,C260,C254), C49(C189,C217,
 C205,C109,C53), C185(C227,C7,C51,C115,C207), N61(C245,C63,C9,C265,C259)
6.e Idealised Me refined as rotating group:
 C282(H28A,H28B,H28C), C361(H36A,H36B,H36C), C219(H21C,H21D,H21E), C95(H95A,
 H95B,H95C), C352(H35C,H35D,H35E), C243(H24A,H24B,H24C), C241(H24D,H24E,H24F),
 C123(H12C,H12D,H12E), C255(H25A,H25B,H25C), C269(H26E,H26F,H26G), C35(H35I,
 H35J,H35K), C41(H41A,H41B,H41C), C331(H33C,H33D,H33E), C81(H81A,H81B,H81C),
 C301(H30A,H30B,H30C), C349(H34E,H34F,H34G), C175(H17E,H17F,H17G), C89(H89A,
 H89B,H89C)
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_smtbx_masks_special_details
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A solvent mask was calculated and 4622 electrons were 
found in a volume of 16109\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
16[C2H3N], 5[C6H14O] per Asymmetric Unit 
which account for 5136 electrons 
per unit cell.
;
_shelx_res_checksum              1956
_shelx_fab_checksum              40057
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'