Complexes of High-Valent Rhenium Supported by the PCP Pincer
Kosanovich, Alex J.; Reibenspies, Joseph H.; Ozerov, Oleg V.; Organometallics 35 (2016) 513–; doi:10.1021/acs.organomet.5b00935

data_4088212
_publ_section_title
;
 Complexes of High-Valent Rhenium Supported by the PCP Pincer
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              513
_journal_paper_doi               10.1021/acs.organomet.5b00935
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C20 H35 Cl2 O P2 Re, 1(C7 H8)'
_chemical_formula_sum            'C27 H43 Cl2 O P2 Re'
_chemical_formula_weight         702.65
_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     direct
_audit_creation_date             2015-11-09
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 93.516(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.9196(10)
_cell_length_b                   14.426(2)
_cell_length_c                   25.637(4)
_cell_measurement_reflns_used    9791
_cell_measurement_temperature    110
_cell_measurement_theta_max      33.575
_cell_measurement_theta_min      2.576
_cell_volume                     2923.5(7)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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_temperature      110.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0637
_diffrn_reflns_av_unetI/netI     0.0452
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            116313
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.858
_diffrn_reflns_theta_min         1.620
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.467
_exptl_absorpt_correction_T_max  0.7468
_exptl_absorpt_correction_T_min  0.4420
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.1235 before and 0.0655 after correction.
The Ratio of minimum to maximum transmission is 0.5919.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.596
_exptl_crystal_description       plate
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.367
_exptl_crystal_size_mid          0.161
_exptl_crystal_size_min          0.086
_refine_diff_density_max         1.786
_refine_diff_density_min         -2.382
_refine_diff_density_rms         0.198
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         12258
_refine_ls_number_restraints     105
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0356
_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^)+(0.0125P)^2^+6.0635P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0606
_refine_ls_wR_factor_ref         0.0666
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9522
_reflns_number_total             12258
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00935_si_002.cif
_cod_data_source_block           reocl
_cod_database_code               4088212
_shelx_estimated_absorpt_t_max   0.700
_shelx_estimated_absorpt_t_min   0.291
_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. Rigid body (RIGU) restrains
 C21, C22, C23, C24, C25, C26, C27, C21A, C22A, C23A, C24A, C25A, C26A, C27A
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
3. Same fragment restrains
{C21, C22, C23, C24, C25, C26, C27} sigma for 1-2: 0.005, 1-3: 0.04
as
{C21A, C22A, C23A, C24A, C25A, C26A, C27A}
4. Others
 Sof(C21A)=Sof(C22A)=Sof(H22A)=Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(H24A)=
 Sof(C25A)=Sof(H25A)=Sof(C26A)=Sof(H26A)=Sof(C27A)=Sof(H27D)=Sof(H27E)=
 Sof(H27F)=1-FVAR(1)
 Sof(C21)=Sof(C22)=Sof(H22)=Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24)=Sof(C25)=
 Sof(H25)=Sof(C26)=Sof(H26)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C1(H1), C12(H12), C15(H15), C18(H18)
5.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C11(H11A,H11B)
5.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26),
 C22A(H22A), C23A(H23A), C24A(H24A), C25A(H25A), C26A(H26A)
5.d Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C27(H27A,H27B,H27C), C27A(H27D,H27E,H27F)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'