Phosphorescent heterobimetallic complexes involving platinum(IV) and rhenium(VII) centers connected by an unsupported μ-oxido bridge
Molaee, Hajar; Nabavizadeh, S. Masoud; Jamshidi, Mahboubeh; Vilsmeier, Max; Pfitzner, Arno; Samandar Sangari, Mozhgan; Dalton Trans.  (2017) –; doi:10.1039/C7DT03126B

data_7044561
_publ_section_title
;
 Phosphorescent heterobimetallic complexes involving platinum(IV) and
 rhenium(VII) centers connected by an unsupported \m-oxido bridge
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT03126B
_journal_year                    2017
_chemical_formula_moiety         'C28 H27 N O4 P Pt Re'
_chemical_formula_sum            'C28 H27 N O4 P Pt Re'
_chemical_formula_weight         853.76
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2016-09-06
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5221)
;
_audit_update_record
;
2017-04-25 deposited with the CCDC.
2017-10-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.8060(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.6078(2)
_cell_length_b                   18.5904(2)
_cell_length_c                   15.4791(2)
_cell_measurement_reflns_used    38635
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      73.4230
_cell_measurement_theta_min      3.7230
_cell_volume                     5291.51(11)
_computing_cell_refinement       'CrysAlisPro 1.171.38.37b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.37b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.37b (Rigaku OD, 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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1773
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -114.00 -13.00   1.00    2.50    --  -41.23 -57.00 120.00  101
  2  \w   -116.00 -17.00   1.00    2.50    --  -41.23 -37.00-150.00   99
  3  \w    -31.00  69.00   1.00    2.50    --   41.23 -57.00  90.00  100
  4  \w     17.00 116.00   1.00    2.50    --   41.23  37.00  30.00   99
  5  \w     24.00 109.00   1.00   10.00    --  106.46 -94.00 120.00   85
  6  \w     77.00 158.00   1.00   10.00    --  106.46  61.00 150.00   81
  7  \w     33.00 121.00   1.00   10.00    --  106.46-125.00  30.00   88
  8  \w     77.00 158.00   1.00   10.00    --  106.46  61.00-150.00   81
  9  \w     74.00 158.00   1.00   10.00    --  106.46  77.00  90.00   84
 10  \w     74.00 158.00   1.00   10.00    --  106.46  77.00 150.00   84
 11  \w     74.00 158.00   1.00   10.00    --  106.46  77.00 120.00   84
 12  \w     73.00 158.00   1.00   10.00    --  106.46 125.00  30.00   85
 13  \w     81.00 158.00   1.00   10.00    --  106.46  45.00 -60.00   77
 14  \w     74.00 158.00   1.00   10.00    --  106.46  77.00   0.00   84
 15  \w     30.00  69.00   1.00   10.00    --  106.46 -30.00   0.00   39
 16  \w     77.00 158.00   1.00   10.00    --  106.46  61.00-180.00   81
 17  \w     73.00 158.00   1.00   10.00    --  106.46 125.00 -90.00   85
 18  \w     30.00  69.00   1.00   10.00    --  106.46 -30.00 150.00   39
 19  \w     74.00 158.00   1.00   10.00    --  106.46  77.00-180.00   84
 20  \w   -117.00  -9.00   1.00    2.50    --  -41.23 -77.00  60.00  108
 21  \w    -66.00  33.00   1.00    2.50    --  -41.23  37.00 -90.00   99
 22  \w      9.00 117.00   1.00    2.50    --   41.23  77.00 -90.00  108
 23  \w      2.00  97.00   1.00    2.50    --   41.23-125.00   0.00   95
 24  \w     74.00 151.00   1.00   10.00    --  106.46  77.00-120.00   77
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0489631000
_diffrn_orient_matrix_UB_12      0.0452081000
_diffrn_orient_matrix_UB_13      0.0507959000
_diffrn_orient_matrix_UB_21      -0.0622642000
_diffrn_orient_matrix_UB_22      -0.0051335000
_diffrn_orient_matrix_UB_23      -0.0777517000
_diffrn_orient_matrix_UB_31      -0.0271988000
_diffrn_orient_matrix_UB_32      -0.0692968000
_diffrn_orient_matrix_UB_33      0.0389723000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_unetI/netI     0.0168
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            59733
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.080
_diffrn_reflns_theta_max         67.080
_diffrn_reflns_theta_min         3.381
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    19.413
_exptl_absorpt_correction_T_max  0.470
_exptl_absorpt_correction_T_min  0.284
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.37b (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.143
_exptl_crystal_description       block
_exptl_crystal_F_000             3216
_exptl_crystal_size_max          0.094
_exptl_crystal_size_mid          0.078
_exptl_crystal_size_min          0.067
_refine_diff_density_max         0.483
_refine_diff_density_min         -0.782
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     655
_refine_ls_number_reflns         9445
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0192
_refine_ls_R_factor_gt           0.0175
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0168P)^2^+6.1759P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0397
_refine_ls_wR_factor_ref         0.0404
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9004
_reflns_number_total             9445
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03126b2.cif
_cod_data_source_block           1_mp_c
_cod_database_code               7044561
_chemical_oxdiff_formula         'C28 H27 N O4 P Pt Re'
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C45(H45), C33(H33), C50(H50), C15(H15), C16(H16), C52(H52), C37(H37),
 C44(H44), C36(H36), C22(H22), C13(H13), C14(H14), C11(H11), C46(H46), C49(H49),
  C43(H43), C53(H53), C35(H35), C39(H39), C17(H17), C12(H12), C34(H34),
 C01K(H01K), C28(H28), C21(H21), C27(H27), C7(H7), C5(H5), C42(H42), C18(H18),
 C41(H41), C9(H9), C26(H26), C8(H8), C40(H40), C6(H6)
2.b Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C1(H1A,H1B,H1C), C3(H3A,H3B,H3C),
 C29(H29A,H29B,H29C), C2(H2A,H2B,H2C)
;
_shelx_res_checksum              70711
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.232
_oxdiff_exptl_absorpt_empirical_full_min 0.858