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_7227874
_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 H17 Br O4 P Re'
_chemical_formula_sum            'C26 H17 Br O4 P Re'
_chemical_formula_weight         690.47
_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             2015-11-10
_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                94.119(4)
_cell_angle_beta                 97.332(4)
_cell_angle_gamma                99.066(4)
_cell_formula_units_Z            2
_cell_length_a                   9.9390(5)
_cell_length_b                   11.0789(5)
_cell_length_c                   11.2433(6)
_cell_measurement_reflns_used    3754
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      28.8690
_cell_measurement_theta_min      3.9980
_cell_volume                     1207.22(11)
_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)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -35.00   59.00   1.0000    3.3500
omega____ theta____ kappa____ phi______ frames
    -      -12.0602   57.0000 -180.0000 94

  2 omega  -77.00   22.00   1.0000    3.3500
omega____ theta____ kappa____ phi______ frames
    -      -12.0602  -77.0000  -90.0000 99

  3 omega  -79.00   14.00   1.0000    3.3500
omega____ theta____ kappa____ phi______ frames
    -      -12.0602  -57.0000   30.0000 93
;
_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      -0.0465512000
_diffrn_orient_matrix_UB_12      0.0148100000
_diffrn_orient_matrix_UB_13      0.0394084000
_diffrn_orient_matrix_UB_21      -0.0001223000
_diffrn_orient_matrix_UB_22      -0.0576638000
_diffrn_orient_matrix_UB_23      0.0236546000
_diffrn_orient_matrix_UB_31      0.0562299000
_diffrn_orient_matrix_UB_32      0.0263855000
_diffrn_orient_matrix_UB_33      0.0443754000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_unetI/netI     0.0693
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7610
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         3.294
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.784
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82720
_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    1.900
_exptl_crystal_description       block
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.156
_refine_diff_density_min         -1.416
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.958
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         4240
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      0.956
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0329
_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^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0571
_refine_ls_wR_factor_ref         0.0608
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3776
_reflns_number_total             4240
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra28263f1.cif
_cod_data_source_block           a151110a
_cod_original_cell_volume        1207.22(10)
_cod_database_code               7227874
_reflns_odcompleteness_completeness 99.74
_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. Restrained distances
 C26-O4
 1.14 with sigma of 0.01
 C27-O5
 1.14 with sigma of 0.01
 Re1-C26
 1.96 with sigma of 0.01
 C27-Re1
 1.96 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C17) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C24) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C26) = Uanis(Br1)
4. Others
 Sof(Br2)=Sof(O4)=Sof(C26)=1-FVAR(1)
 Sof(Br1)=Sof(O5)=Sof(C27)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C6(H6), C7(H7), C8(H8), C9(H9), C12(H12), C13(H13),
 C14(H14), C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2015-11-10
_olex2_submission_special_instructions 'No special instructions were received'