Impact of the Alkyne Substitution Pattern and Metalation on the Photoisomerization of Azobenzene-Based Platinum(II) Diynes and Polyynes.
Al-Balushi, Rayya A; Haque, Ashanul; Jayapal, Maharaja; Al-Suti, Mohammed K; Husband, John; Khan, Muhammad S.; Skelton, Jonathan M.; Molloy, Kieran C.; Raithby, Paul R.; Inorganic chemistry 55 (2016) 10955–10967; doi:10.1021/acs.inorgchem.6b01509

data_4348673
_publ_section_title
;
 Impact of the Alkyne Substitution Pattern and Metalation on the
 Photoisomerization of Azobenzene-Based Platinum(II) Diynes and Polyynes.
;
_journal_issue                   21
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10955
_journal_page_last               10967
_journal_paper_doi               10.1021/acs.inorgchem.6b01509
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C52 H78 N2 P4 Pt2'
_chemical_formula_sum            'C52 H78 N2 P4 Pt2'
_chemical_formula_weight         1245.22
_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     iterative
_audit_creation_date             2016-06-15
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 110.929(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.7794(4)
_cell_length_b                   10.5232(2)
_cell_length_c                   14.8114(3)
_cell_measurement_reflns_used    23665
_cell_measurement_temperature    150
_cell_measurement_theta_max      30.5600
_cell_measurement_theta_min      3.6590
_cell_volume                     2733.91(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0734
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_details
;
  1 omega  -47.00   37.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       20.1293  -57.0000  -90.0000 84

  2 omega   -7.00   88.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       20.1293   77.0000 -180.0000 95

  3 omega    3.00   87.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       20.1293   57.0000   30.0000 84

  4 omega  -47.00   47.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       20.1293  -77.0000   60.0000 94

  5 omega    3.00   87.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       20.1293   57.0000  -60.0000 84

  6 omega    3.00   87.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       20.1293   57.0000   90.0000 84

  7 omega  -20.00   59.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       20.1293  -99.0000  -30.0000 79

  8 omega  -20.00   59.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       20.1293  -99.0000 -180.0000 79

  9 omega   35.00   92.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       20.1293  178.0000  -30.0000 57

 10 omega   35.00   92.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       20.1293  178.0000  -90.0000 57

 11 omega  -91.00  -35.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.1918 -178.0000    0.0000 56

 12 omega   10.00   81.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       20.1293 -138.0000  -51.0000 71

 13 omega    6.00   47.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       20.1293 -132.0000  125.0000 41

 14 omega  -49.00   39.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       20.1293  -38.0000  -60.0000 88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0379205000
_diffrn_orient_matrix_UB_12      -0.0213228000
_diffrn_orient_matrix_UB_13      0.0103302000
_diffrn_orient_matrix_UB_21      -0.0140029000
_diffrn_orient_matrix_UB_22      -0.0560767000
_diffrn_orient_matrix_UB_23      -0.0270876000
_diffrn_orient_matrix_UB_31      0.0007493000
_diffrn_orient_matrix_UB_32      0.0307374000
_diffrn_orient_matrix_UB_33      -0.0422825000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.941
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            70107
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.979
_diffrn_reflns_theta_min         3.366
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.262
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65287
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_description       block
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   1.0000
_exptl_transmission_factor_min   0.65287
_refine_diff_density_max         1.370
_refine_diff_density_min         -0.769
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         8186
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0287
_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^)+(0.0184P)^2^+2.5070P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0508
_refine_ls_wR_factor_ref         0.0533
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7002
_reflns_number_total             8186
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01509_si_002.cif
_cod_data_source_block           e14prr9
_cod_original_cell_volume        2733.89(11)
_cod_database_code               4348673
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C75 H114 N1 P4 Pt4'
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_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.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C11(H11A,H11B), C13(H13A,H13B), C15(H15A,H15B), C17(H17A,H17B),
 C19(H19A,H19B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C8(H8), C22(H22), C23(H23), C24(H24), C25(H25),
 C26(H26)
2.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C16(H16A,H16B,
 H16C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              15939
_shelx_hkl_checksum              71366
_olex2_date_sample_data_collection 1415454708.0
_olex2_exptl_crystal_mounting_method
'Fluoroether oil in a nitrogen cold stream'
_olex2_submission_original_sample_id e14prr9
_olex2_submission_special_instructions 'No special instructions were received'