Three-Fold Intramolecular Ring Closing Alkene Metatheses of Square Planar Complexes with cis Phosphorus Donor Ligands P(X(CH<sub>2</sub>) <sub>m</sub>CH═CH<sub>2</sub>)<sub>3</sub> (X = -, m = 5-10; X = O, m = 3-5): Syntheses, Structures, and Thermal Properties of Macrocyclic Dibridgehead Diphosphorus Complexes.
Joshi, Hemant; Kharel, Sugam; Ehnbom, Andreas; Skopek, Katrin; Hess, Gisela D.; Fiedler, Tobias; Hampel, Frank; Bhuvanesh, Nattamai; Gladysz, John A.; Journal of the American Chemical Society 140 (2018) 8463–8478; doi:10.1021/jacs.8b02846

data_4132283
_publ_section_title
;
 Three-Fold Intramolecular Ring Closing Alkene Metatheses of Square Planar
 Complexes with cis Phosphorus Donor Ligands P(X(CH<sub>2</sub>)
 <sub>m</sub>CH&#x2550;CH<sub>2</sub>)<sub>3</sub> (X = -, m = 5-10; X =
 O, m = 3-5): Syntheses, Structures, and Thermal Properties of Macrocyclic
 Dibridgehead Diphosphorus Complexes.
;
_journal_issue                   27
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8463
_journal_page_last               8478
_journal_paper_doi               10.1021/jacs.8b02846
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C66 H126 Cl2 P2 Pt'
_chemical_formula_sum            'C66 H126 Cl2 P2 Pt'
_chemical_formula_weight         1247.59
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-05-04
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_cell_angle_alpha                90
_cell_angle_beta                 95.492(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.469(2)
_cell_length_b                   13.8800(12)
_cell_length_c                   20.2636(18)
_cell_measurement_reflns_used    9884
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      65.251
_cell_measurement_theta_min      3.628
_cell_volume                     6850.5(10)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0685
_diffrn_reflns_av_unetI/netI     0.0515
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            32664
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        49.998
_diffrn_reflns_theta_max         49.998
_diffrn_reflns_theta_min         3.629
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.235
_exptl_absorpt_correction_T_max  0.8303
_exptl_absorpt_correction_T_min  0.3770
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1226 before and 0.0839 after correction. The Ratio of minimum to maximum transmission is 0.4541. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_description       plate
_exptl_crystal_F_000             2656
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.108
_exptl_crystal_size_min          0.037
_refine_diff_density_max         1.530
_refine_diff_density_min         -0.692
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     668
_refine_ls_number_reflns         6880
_refine_ls_number_restraints     136
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0550
_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^)+74.6253P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1128
_refine_ls_wR_factor_ref         0.1260
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5699
_reflns_number_total             6880
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b02846_si_003.cif
_cod_data_source_block           sk600a
_cod_original_cell_volume        6850.6(11)
_cod_database_code               4132283
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.830
_shelx_estimated_absorpt_t_min   0.406
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 C33-C32 \\sim C22-C21 \\sim C44-C43 \\sim C32A-C33A
 with sigma of 0.01
 C32-C31 \\sim C21-C20 \\sim C43-C42 \\sim C11-C10 \\sim C66-C65 \\sim C55-C54
 with sigma of 0.01
 C31-C30 \\sim C31A-C30
 with sigma of 0.01
 C32-C31 \\sim C32A-C31A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C30 \\sim C31 \\sim C32 \\sim C33 \\sim C31A \\sim C32A \\sim C33A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C30, C31, C32, C33, C31A, C32A, C33A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Others
 Sof(H30C)=Sof(H30D)=Sof(C31A)=Sof(H31C)=Sof(H31D)=Sof(C32A)=Sof(H32A)=
 Sof(C33A)=Sof(H33C)=Sof(H33D)=1-FVAR(1)
 Sof(H30A)=Sof(H30B)=Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(C32)=Sof(H32)=Sof(C33)=
 Sof(H33A)=Sof(H33B)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C12(H12A,H12B), C13(H13A,H13B),
 C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B),
  C19(H19A,H19B), C20(H20A,H20B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,
 H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B),
 C30(H30A,H30B), C30(H30C,H30D), C31(H31A,H31B), 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), 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), C56(H56A,H56B), C57(H57A,H57B), C58(H58A,
 H58B), C59(H59A,H59B), C60(H60A,H60B), C61(H61A,H61B), C62(H62A,H62B),
 C63(H63A,H63B), C64(H64A,H64B), C31A(H31C,H31D)
6.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C21(H21), C32(H32), C43(H43), C54(H54), C65(H65), C32A(H32A)
6.c X=CH2 refined with riding coordinates:
 C11(H11A,H11B), C22(H22A,H22B), C33(H33A,H33B), C44(H44A,H44B), C55(H55A,
 H55B), C66(H66A,H66B), C33A(H33C,H33D)
;
_shelx_res_checksum              29746
_shelx_hkl_checksum              64032
_olex2_submission_special_instructions 'No special instructions were received'