Synthesis of geometry-controlled platinum-containing polymers bearing optically active bidentate phosphine ligands
Horiuchi, Takashi; Makino, Soya; Sano, Natsuhiro; Sogawa, Hiromitsu; Sanda, Fumio; Polymer Chemistry 15 (2024) 303–309; doi:10.1039/D3PY01074K

data_1570555
_publ_section_title
;
 Synthesis of geometry-controlled platinum-containing polymers bearing
 optically active bidentate phosphine ligands
;
_journal_issue                   4
_journal_name_full               'Polymer Chemistry'
_journal_page_first              303
_journal_page_last               309
_journal_paper_doi               10.1039/D3PY01074K
_journal_volume                  15
_journal_year                    2024
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C70 H60 N2 O6 P2 Pt'
_chemical_formula_sum            'C70 H60 N2 O6 P2 Pt'
_chemical_formula_weight         1282.23
_space_group_crystal_system      tetragonal
_space_group_IT_number           92
_space_group_name_Hall           'P 4abw 2nw'
_space_group_name_H-M_alt        'P 41 21 2'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc2fd2b8
_audit_creation_date             2021-09-13
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6396)
;
_audit_update_record
;
2023-03-19 deposited with the CCDC.	2023-12-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.4819(13)
_cell_length_b                   23.4819(13)
_cell_length_c                   33.2671(9)
_cell_measurement_reflns_used    65883
_cell_measurement_temperature    123.00
_cell_measurement_theta_max      54.98
_cell_measurement_theta_min      3.47
_cell_volume                     18343.5(15)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      123.00
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'RIGAKU RAPID-II'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_unetI/netI     0.0607
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            102569
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         2.449
_diffrn_source_current           100.0
_diffrn_source_power             5.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.600
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4768
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    0.929
_exptl_crystal_description       block
_exptl_crystal_F_000             5200
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.507
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.093(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     713
_refine_ls_number_reflns         20512
_refine_ls_number_restraints     475
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0976
_refine_ls_R_factor_gt           0.0500
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0751P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1198
_refine_ls_wR_factor_ref         0.1365
_reflns_Friedel_coverage         0.803
_reflns_Friedel_fraction_full    0.967
_reflns_Friedel_fraction_max     0.963
_reflns_number_gt                11793
_reflns_number_total             20512
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3py01074k2.cif
_cod_data_source_block           shelx_sq_sq_sq
_cod_depositor_comments          'Adding full bibliography for 1570555.cif.'
_cod_original_cell_volume        18343(2)
_cod_database_code               1570555
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.856
_shelx_estimated_absorpt_t_min   0.502
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.907(9)
 0.093(9)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C1E-C2E = C2E-C3E = C3E-C4E = C4E-C5E = C5E-C6E = C6E-C1E
 1.38 with sigma of 0.02
 C4I-C9I = C9I-C10I = C9I-C10I
 1.52 with sigma of 0.02
 C6G-C9G
 1.5 with sigma of 0.02
 C9G-C10G
 1.2 with sigma of 0.01
 C1B-C2B = C2B-C3B = C3B-C4B = C4B-C5B = C5B-C6B = C6B-C1B
 1.38 with sigma of 0.02
 C3G-C4G = C4G-C5G = C5G-C6G = C6G-C7G = C7G-C8G = C8G-C3G
 1.38 with sigma of 0.02
 C1D-C2D = C2D-C3D = C3D-C4D = C4D-C5D = C5D-C6D = C6D-C1D
 1.38 with sigma of 0.02
 N3I-C4I
 1.47 with sigma of 0.02
 C4I-C5I
 1.54 with sigma of 0.02
 N3J-C4J
 1.47 with sigma of 0.02
 C4J-C5J
 1.54 with sigma of 0.02
 C1A-C2A = C2A-C3A = C3A-C4A = C4A-C5A = C5A-C6A = C6A-C1A
 1.38 with sigma of 0.02
 C5I-O6I
 1.21 with sigma of 0.02
 C5I-O7I
 1.37 with sigma of 0.02
 C4J-C9J = C9J-C10J = C9J-C11J
 1.54 with sigma of 0.02
 O7J-C8J = O7I-C8I
 1.43 with sigma of 0.02
 C1I-N3I
 1.47 with sigma of 0.02
 C4C-C1I
 1.54 with sigma of 0.02
 C8J-C8I
 1.54 with sigma of 0.02
 C1I-O2I
 1.22 with sigma of 0.02
 C5I-C9I = C4I-C10I = C4I-C11I
 2.44 with sigma of 0.04
 C9G-C10G
 2.7 with sigma of 0.04
 C5G-C9G = C7G-C9G
 2.51 with sigma of 0.04
 C1B-C3B = C2B-C4B = C3B-C5B = C4B-C6B = C5B-C1B = C6B-C2B
 2.39 with sigma of 0.04
 C3G-C5G = C4G-C6G = C5G-C7G = C6G-C8G = C7G-C3G = C8G-C4G
 2.39 with sigma of 0.04
 C4J-O7J
 2.57 with sigma of 0.04
 C1E-C3E = C2E-C4E = C3E-C5E = C4E-C6E = C5E-C1E = C6E-C2E
 2.39 with sigma of 0.04
 C1D-C3D = C2D-C4D = C3D-C5D = C4D-C6D = C5D-C1D = C6D-C2D
 2.39 with sigma of 0.04
 C5J-C8J
 2.27 with sigma of 0.04
 N3J-C5J
 2.61 with sigma of 0.04
 N3I-C5I
 2.61 with sigma of 0.04
 C4I-O6I
 2.35 with sigma of 0.04
 C4J-O6J
 2.4 with sigma of 0.04
 C1A-C3A = C2A-C4A = C3A-C5A = C4A-C6A = C5A-C1A = C6A-C2A
 2.39 with sigma of 0.04
 C4I-O7I
 2.49 with sigma of 0.04
 C5J-C9J = C4J-C10J = C4J-C11J
 2.44 with sigma of 0.04
 C5I-C8I
 2.22 with sigma of 0.04
 O7J-C8I = O7I-C8J
 2.35 with sigma of 0.04
 C4C-N3I
 2.61 with sigma of 0.04
 O2I-N3I
 2.33 with sigma of 0.04
 C4C-O2I
 2.4 with sigma of 0.04
4. Restrained planarity
 C1G, C2G, C3G, C4G, C5G, C6G, C7G, C8G, C9G, C10G
 with sigma of 0.1
 C1B, C2B, C3B, C4B, C5B, C6B
 with sigma of 0.1
 C1E, C2E, C3E, C4E, C5E, C6E
 with sigma of 0.1
 C4J, C5J, O6J, O7J
 with sigma of 0.1
 C1D, C2D, C3D, C4D, C5D, C6D
 with sigma of 0.1
 C1A, C2A, C3A, C4A, C5A, C6A
 with sigma of 0.1
 C4I, C5I, O6I, O7I
 with sigma of 0.1
 C4C, C1I, O2I, N3I
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
Uanis(C1I) \\sim Ueq, Uanis(O2I) \\sim Ueq, Uanis(N3I) \\sim Ueq, Uanis(C4I)
\\sim Ueq, Uanis(C5I) \\sim Ueq, Uanis(O6I) \\sim Ueq, Uanis(O7I) \\sim Ueq,
Uanis(C8I) \\sim Ueq, Uanis(C9I) \\sim Ueq, Uanis(C10I) \\sim Ueq, Uanis(C11I)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1J) \\sim Ueq, Uanis(O2J) \\sim Ueq, Uanis(N3J) \\sim Ueq, Uanis(C4J)
\\sim Ueq, Uanis(C5J) \\sim Ueq, Uanis(O6J) \\sim Ueq, Uanis(O7J) \\sim Ueq,
Uanis(C8J) \\sim Ueq, Uanis(C9J) \\sim Ueq, Uanis(C10J) \\sim Ueq, Uanis(C11J)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C4I) = Uanis(C5I) = Uanis(O6I) = Uanis(O7I)
6. Rigid body (RIGU) restrains
 C1G, C2G, C3G, C4G, C5G, C6G, C7G, C8G, C9G, C10G
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C9I, C10I
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C1B, C2B, C3B, C4B, C5B, C6B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C1E, C2E, C3E, C4E, C5E, C6E
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C1D, C2D, C3D, C4D, C5D, C6D
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C1A, C2A, C3A, C4A, C5A, C6A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 N3I, C4I
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C9J, C10J
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
7.a Ternary CH refined with riding coordinates:
 C4J(H4J), C4I(H4I), C9I(H9I), C9J(H9J)
7.b Secondary CH2 refined with riding coordinates:
 C8J(H8JA,H8JB), C8I(H8IA,H8IB)
7.c Me refined with riding coordinates:
 C11I(H11A,H11B,H11C), C10I(H10A,H10B,H10C), C10J(H10D,H10E,H10F), C11J(H11D,
 H11E,H11F)
7.d Aromatic/amide H refined with riding coordinates:
 C6D(H6D), C3F(H3F), C6C(H6C), C4E(H4E), C2A(H2A), C3C(H3C), C5A(H5A),
 C5F(H5F), C3B(H3B), C5D(H5D), C2B(H2B), C2E(H2E), C2C(H2C), C3E(H3E), C4B(H4B),
  C5C(H5C), C3A(H3A), C2F(H2F), C4A(H4A), C6A(H6A), C5B(H5B), C6B(H6B),
 C4D(H4D), C5E(H5E), C6E(H6E), C2D(H2D), C3D(H3D), C40(H40), C43(H43), C39(H39),
  C42(H42), C4G(H4G), C8G(H8G), N3I(H3I), N3J(H3J), C5G(H5G), C7G(H7G), C6F(H6F)
7.e :
 C45(H45), C10G(H10G)
;
_shelx_res_checksum              2657
_shelx_fab_checksum              24146
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'