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_7227875
_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         'C28 H17 F3 O6 P Re'
_chemical_formula_sum            'C28 H17 F3 O6 P Re'
_chemical_formula_weight         723.58
_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
_audit_creation_date             2016-06-21
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-12-05 deposited with the CCDC.
2017-03-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.995(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.3119(9)
_cell_length_b                   11.3315(3)
_cell_length_c                   19.6695(6)
_cell_measurement_reflns_used    14815
_cell_measurement_temperature    154.5(9)
_cell_measurement_theta_max      29.4040
_cell_measurement_theta_min      3.7940
_cell_volume                     5352.1(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (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      154.5(9)
_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 0.998
_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     -7.00  28.00   1.00    7.21    --   11.08  19.00 120.00   35
  2  \w     46.00  89.00   1.00    7.21    --   11.08  19.00 120.00   43
  3  \w      0.00  75.00   1.00    7.21    --   11.08  57.00 -30.00   75
  4  \w    -13.00  84.00   1.00    7.21    --   11.08  38.00-150.00   97
  5  \w    -10.00  30.00   1.00    7.21    --  -11.24 -99.00-180.00   40
  6  \w    -61.00 -33.00   1.00    7.21    --   11.08 -38.00-120.00   28
  7  \w    -20.00  45.00   1.00    7.21    --   11.08 -99.00  60.00   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_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0287137000
_diffrn_orient_matrix_UB_12      0.0146687000
_diffrn_orient_matrix_UB_13      -0.0049802000
_diffrn_orient_matrix_UB_21      -0.0002866000
_diffrn_orient_matrix_UB_22      -0.0066507000
_diffrn_orient_matrix_UB_23      0.0358047000
_diffrn_orient_matrix_UB_31      0.0069430000
_diffrn_orient_matrix_UB_32      0.0604758000
_diffrn_orient_matrix_UB_33      0.0051359000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0564
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            45685
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         3.409
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.662
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.29253
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
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    1.796
_exptl_crystal_description       block
_exptl_crystal_F_000             2800
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.915
_refine_diff_density_min         -1.425
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         9416
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0487
_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^)+(0.0350P)^2^+54.6661P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1086
_refine_ls_wR_factor_ref         0.1129
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8278
_reflns_number_total             9416
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra28263f1.cif
_cod_data_source_block           a160617c
_cod_database_code               7227875
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(F2) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(F4) \\sim
Ueq, Uanis(F5) \\sim Ueq, Uanis(F6) \\sim Ueq: with sigma of 0.005 and sigma
for terminal atoms of 0.002
Uanis(C18) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C22)
\\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C5) \\sim Ueq,
Uanis(C4) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C2) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.002
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C13(H13),
 C14(H14), C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22),
  C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C37(H37), C38(H38),
 C39(H39), C40(H40), C42(H42), C43(H43), C44(H44), C46(H46), C47(H47), C48(H48),
  C49(H49), C50(H50)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-06-17
_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 2.596
_oxdiff_exptl_absorpt_empirical_full_min 0.540