Synthesis, structures and catalytic activity of cyclometalated rhenium complexes
Sun, Ruichen; Wang, Tian; Zhang, Shaowei; Chu, Xiaodan; Zhu, Bolin; RSC Adv. 7 (2017) 17063–; doi:10.1039/C6RA28263F

data_7227872
_publ_section_title
;
 Synthesis, structures and catalytic activity of cyclometalated rhenium
 complexes
;
_journal_issue                   28
_journal_name_full               'RSC Adv.'
_journal_page_first              17063
_journal_paper_doi               10.1039/C6RA28263F
_journal_volume                  7
_journal_year                    2017
_chemical_formula_moiety         'C26 H16 O4 P Re'
_chemical_formula_sum            'C26 H16 O4 P Re'
_chemical_formula_weight         609.56
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-10-29
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4959)
;
_audit_update_record
;
2016-12-05 deposited with the CCDC.
2017-03-14 downloaded from the CCDC.
;
_cell_angle_alpha                64.239(2)
_cell_angle_beta                 84.8034(19)
_cell_angle_gamma                74.8834(19)
_cell_formula_units_Z            4
_cell_length_a                   11.9989(3)
_cell_length_b                   14.4984(3)
_cell_length_c                   14.8134(4)
_cell_measurement_reflns_used    11817
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      74.1120
_cell_measurement_theta_min      4.4930
_cell_volume                     2239.82(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2740
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_details
;
  1 omega  -45.00   31.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000  -30.0000 76

  2 omega  -35.00   -9.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  125.0000  -30.0000 26

  3 omega  -92.00   -4.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  125.0000   30.0000 88

  4 omega -110.00  -23.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -38.0000 -180.0000 87

  5 omega  -54.00  -22.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -38.0000   90.0000 32

  6 omega   52.00   97.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1514 -125.0000    0.0000 45

  7 omega   47.00  121.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      106.0351 -125.0000  -30.0000 74

  8 omega  103.00  145.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      106.0351  -15.0000 -150.0000 42

  9 omega  141.00  173.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      106.0351   45.0000 -150.0000 32

 10 omega   96.00  123.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      106.0351  125.0000 -120.0000 27

 11 omega   93.00  137.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      106.0351   45.0000 -150.0000 44

 12 omega   38.00   76.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      106.0351  -30.0000 -180.0000 38

 13 omega   33.00   86.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      106.0351  -30.0000  -90.0000 53

 14 omega   40.00  135.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      106.0351  -77.0000  -30.0000 95

 15 omega   87.00  120.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      106.0351 -125.0000 -180.0000 33

 16 omega   33.00   81.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      106.0351  -30.0000  -30.0000 48

 17 omega   33.00   88.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      106.0351  -30.0000   30.0000 55

 18 omega   34.00   90.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      106.0351  -30.0000   90.0000 56

 19 omega   36.00  136.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      106.0351  -77.0000  120.0000 100

 20 omega   31.00   96.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      106.0351  -15.0000 -150.0000 65
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.1087996000
_diffrn_orient_matrix_UB_12      0.0756831000
_diffrn_orient_matrix_UB_13      0.0151975000
_diffrn_orient_matrix_UB_21      -0.0324852000
_diffrn_orient_matrix_UB_22      0.0468753000
_diffrn_orient_matrix_UB_23      -0.1121936000
_diffrn_orient_matrix_UB_31      -0.0693320000
_diffrn_orient_matrix_UB_32      -0.0830548000
_diffrn_orient_matrix_UB_33      0.0229149000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16330
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.364
_diffrn_reflns_theta_min         3.314
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.544
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40918
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.808
_exptl_crystal_description       block
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.880
_refine_diff_density_min         -0.991
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         8839
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_gt           0.0294
_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^)+(0.0443P)^2^+1.6094P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0764
_refine_ls_wR_factor_ref         0.0780
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8300
_reflns_number_total             8839
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra28263f1.cif
_cod_data_source_block           a151027b
_cod_database_code               7227872
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13),
 C14(H14), C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22),
  C30(H30), C31(H31), C32(H32), C34(H34), C35(H35), C36(H36), C38(H38),
 C39(H39), C40(H40), C41(H41), C42(H42), C44(H44), C45(H45), C46(H46), C47(H47),
  C48(H48)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2015-10-27
_olex2_submission_special_instructions 'No special instructions were received'