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_7711469
_publ_section_title
;
 cis-Dipyridyl Porphyrin-Based Multicomponent Organoplatinum(II)
 Bismetallacycles for Photocatalytic Oxidation
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02197H
_journal_year                    2022
_chemical_formula_moiety
'2(C77 H91 N6 O4 P4 Pt2), 13[C2H3N], 5[C6H14O], 0.5[], 1[], 0.5[]'
_chemical_formula_sum            'C210 H291 N25 O13 P8 Pt4'
_chemical_formula_weight         4401.78
_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 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2022-10-09 deposited with the CCDC.	2022-10-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 134.806(19)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   53.469(13)
_cell_length_b                   26.692(6)
_cell_length_c                   37.842(10)
_cell_measurement_reflns_used    6776
_cell_measurement_temperature    193.0
_cell_measurement_theta_max      41.42
_cell_measurement_theta_min      2.68
_cell_volume                     38318(2)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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      193.0
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.998
_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  0.1181
_diffrn_reflns_av_unetI/netI     0.0740
_diffrn_reflns_Laue_measured_fraction_full 0.961
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       63
_diffrn_reflns_limit_h_min       -63
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            211404
_diffrn_reflns_point_group_measured_fraction_full 0.961
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.901
_diffrn_reflns_theta_min         0.933
_exptl_absorpt_coefficient_mu    3.048
_exptl_absorpt_correction_T_max  0.7506
_exptl_absorpt_correction_T_min  0.5881
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1206 before and 0.0869 after correction.
The Ratio of minimum to maximum transmission is 0.7835.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_description       block
_exptl_crystal_F_000             18096
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.221
_refine_diff_density_min         -1.333
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1566
_refine_ls_number_reflns         33330
_refine_ls_number_restraints     3540
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.1494
_refine_ls_R_factor_gt           0.0973
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+10.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2944
_refine_ls_wR_factor_ref         0.3440
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16381
_reflns_number_total             33330
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02197h2.cif
_cod_data_source_block           123_sq
_cod_original_cell_volume        38319(18)
_cod_database_code               7711469
_shelxl_version_number           2014-1
_shelx_estimated_absorpt_t_max   0.750
_shelx_estimated_absorpt_t_min   0.675
_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
 H21C-H28A
 2.1 with sigma of 0.02
 H61-H9
 2.1 with sigma of 0.02
 HQ-H65
 2.1 with sigma of 0.02
 H13E-H33A
 2.1 with sigma of 0.02
 H66-HQ
 2.1 with sigma of 0.02
 H10B-H13F
 2.1 with sigma of 0.02
 H35D-H35A
 2.1 with sigma of 0.02
 H35C-H53_$1
 2.1 with sigma of 0.02
 C313-C261
 3.1 with sigma of 0.01
 C273-C343
 3.1 with sigma of 0.01
 C343-C273
 3.95 with sigma of 0.01
 C273-C270
 3.3 with sigma of 0.01
 C239-C217
 3.5 with sigma of 0.01
 C119_$1-C350
 3.5 with sigma of 0.01
 C350-C13
 3.3 with sigma of 0.01
 C135-C233
 3.3 with sigma of 0.01
 C280-C33
 3.8 with sigma of 0.01
 C33-C133
 1.53 with sigma of 0.01
 C33-C280
 3.9 with sigma of 0.01
 P26-C33
 2.7 with sigma of 0.01
 C297-C173 \\sim C250-C208 \\sim C80-C232 \\sim C166-C106 \\sim C192-C127 \\sim
C88-C114 \\sim C212-
 C143 \\sim C29-C125
 with sigma of 0.0008
 C212-C204 \\sim C322-C212 \\sim C192-C140 \\sim C192-C170 \\sim C152-C114
\\sim C68-C114 \\sim C29-
 C186 \\sim C79-C29 \\sim C266-C208 \\sim C230-C208 \\sim C302-C297 \\sim
C323-C297 \\sim C80-C150 ~
 C80-C78 \\sim C166-C122 \\sim C60-C166
 with sigma of 0.0008
 C83-C79 \\sim C83-C317 \\sim C317-C140 \\sim C74-C170 \\sim C74-C66 \\sim
C66-C152 \\sim C190-C186 ~
 C324-C190 \\sim C324-C322 \\sim C303-C204 \\sim C320-C303 \\sim C68-C320 \\sim
C230-C196 \\sim C316-
 C196 \\sim C316-C302 \\sim C323-C206 \\sim C244-C206 \\sim C244-C150 \\sim
C78-C160 \\sim C222-C160 ~
 C60-C222 \\sim C226-C122 \\sim C242-C226 \\sim C266-C242
 with sigma of 0.0008
 P24-C220 \\sim P24-C95 \\sim P24-C313 \\sim P12-C262 \\sim P12-C43 \\sim
P12-C337 \\sim P40-C13 \\sim P40-
 C177 \\sim P40-C357 \\sim P18-C193 \\sim P18-C135 \\sim P18-C340 \\sim
P26-C321 \\sim P26-C133 \\sim P26-
 C213 \\sim P38-C280 \\sim P38-C307 \\sim P38-C331 \\sim P8-C270 \\sim P8-C319
\\sim P8-C343 \\sim P14-C273
 \\sim P14-C284 \\sim P14-C169
 with sigma of 0.001
 C79-C65 \\sim C186-C119
 with sigma of 0.0008
 C65-C29 \\sim C29-C119
 with sigma of 0.0008
 C31-C284 \\sim C273-C239 \\sim C352-C169 \\sim C7-C343 \\sim C270-C217 \\sim
C319-C305 \\sim C331-
 C181 \\sim C307-C215 \\sim C280-C103 \\sim C33-C133 \\sim C45-C213 \\sim
C321-C109 \\sim C95-C261 ~
 C313-C223 \\sim C220-C111 \\sim C43-C346 \\sim C51-C337 \\sim C262-C167 \\sim
C340-C233 \\sim C73-C193
 \\sim C135-C113 \\sim C99-C357 \\sim C145-C13 \\sim C350-C177
 with sigma of 0.0008
 O52-C82 \\sim O50-C82 \\sim O132-C116 \\sim O20-C116 \\sim O32-C130 \\sim
O48-C130 \\sim O30-C144 ~
 O42-C144
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C273 \\sim C239: within 1.8A with sigma of 0.005 and sigma for terminal atoms
of 0.01
C340 \\sim C233: within 1.8A with sigma of 0.005 and sigma for terminal atoms
of 0.01
C133 \\sim C33: within 1.8A with sigma of 0.005 and sigma for terminal atoms of
0.01
All non-hydrogen atoms have similar U: within -2.7A with sigma of 0.009 and
sigma for terminal atoms of 0.018
Uanis(C33) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4.a Riding coordinates:
 C305(H14,H15,H16), C7(H17,H18,H19), C352(H24,H25,H26), C109(H10A,H10B,H10C),
 C103(H10D,H10E,H10F), C111(H30,H31,H32), C223(H33,H34,H35), C350(H35C,H35D,
 H35E), C73(H73A,H73B,H73C), C145(H14A,H14B,H14C), C261(H58,H59,H60), C33(H33C,
 H33D,H33E), C233(H23A,H23B,H23C)
4.b Secondary CH2 refined with riding coordinates:
 C262(HN,HO), C270(HP,HQ), C280(H28A,H28B), C284(HR,HS), C220(HT,HU),
 C307(H30A,H30B), C321(H32A,H32B), C319(HV,HW), C313(HX,HY), C357(H35A,H35B),
 C337(HZ,H1), C43(H4,H5), C169(H7,H8), C343(H9,H10), C331(H33A,H33B), C177(H17A,
 H17B), C213(H21D,H21E), C340(H34A,H34B), C95(H39,H40), C193(H19A,H19B),
 C13(H13A,H13B), C135(H13C,H13D), C133(H13E,H13F), C273(H61,H63)
4.c Aromatic/amide H refined with riding coordinates:
 C164(H), C118(HA), C126(HB), C70(HC), C96(H96), C142(H142), C158(H158),
 C138(H138), C124(HD), C4(HE), C134(HF), C92(H92), C62(H62), C146(H146),
 C160(H160), C66(HG), C74(HH), C190(HI), C324(HJ), C320(HK), C294(H294),
 C228(H228), C240(H240), C224(H224), C198(HL), C222(H222), C226(H226),
 C242(H242), C244(H244), C296(HM), C252(H252), C194(H194), C274(H274),
 C254(H254), C306(H306), C196(H196), C268(H268), C308(H308), C316(H316),
 C206(H206), C157(H157), C21(H21), C335(H335), C301(H301), C77(H77), C303(H2),
 C83(H3), C317(H6), C289(H44), C263(H45), C2(H46), C139(H47), C137(H48),
 C277(H49), C267(H50), C253(H51), C363(H52), C119(H53), C257(H54), C141(H55),
 C115(H56), C65(H57)
4.d Fitted hexagon refined as free rotating group:
 N22(C164,C118,C88,C126,C70), N28(C96,C142,C106,C158,C138), C10(C124,C100,C4,
 C120,C134), C92(C108,C62,C176,C146,C136), C232(C294,C228,N314,C240,C224),
 C250(C252,C194,C274,C254,C306), C173(C157,C21,C335,C301,C77), C143(C289,C263,
 C2,C139,C137), C127(C277,C267,N129,C253,C363), C125(C119,C257,C141,C115,C65)
4.e Idealised Me refined as rotating group:
 C167(H11,H12,H13), C45(H45A,H45B,H45C), C181(H18A,H18B,H18C), C215(H21A,H21B,
 H21C), C217(H20,H22,H23), C51(H27,H28,H29), C346(H36,H37,H38), C99(H99A,H99B,
 H99C), C113(H11A,H11B,H11C), C31(H41,H42,H43), C239(H64,H65,H66)
;
_shelx_res_checksum              15315
_platon_squeeze_special_details
;
A solvent mask was calculated and 4190 electrons were 
found in a volume of 17368\%A^3^ in 4 voids per unit cell. 
This is consistent with the presence of 
13[C2H3N], 5[C6H14O], per Asymmetric Unit 
which account for 4608 electrons 
per unit cell.
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'