Synthesis, characterization, kinetic investigation and biological evaluation of Re(i) di- and tricarbonyl complexes with tertiary phosphine ligands.
Gantsho, Verity Lindy; Dotou, Mazzarine; Jakubaszek, Marta; Goud, Bruno; Gasser, Gilles; Visser, Hendrik Gideon; Schutte-Smith, Marietjie; Dalton transactions (Cambridge, England : 2003) 49 (2020) 35–46; doi:10.1039/c9dt04025k

data_7701886
_publ_section_title
;
 Synthesis, characterization, kinetic investigation and biological
 evaluation of Re(i) di- and tricarbonyl complexes with tertiary phosphine
 ligands.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              35
_journal_page_last               46
_journal_paper_doi               10.1039/c9dt04025k
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C45 H35 O4 P2 Re, 2(C7 H8)'
_chemical_formula_sum            'C59 H51 O4 P2 Re'
_chemical_formula_weight         1072.14
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-08-13
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-08-16 deposited with the CCDC.	2019-11-07 downloaded from the CCDC.
;
_cell_angle_alpha                66.491(3)
_cell_angle_beta                 72.612(6)
_cell_angle_gamma                75.940(6)
_cell_formula_units_Z            2
_cell_length_a                   11.144(2)
_cell_length_b                   14.985(3)
_cell_length_c                   16.723(3)
_cell_measurement_reflns_used    9742
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.93
_cell_measurement_theta_min      3.95
_cell_volume                     2419.3(8)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0547
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            72929
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         1.497
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.626
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6318
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0768 before and 0.0643 after correction.
The Ratio of minimum to maximum transmission is 0.8473.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_description       Cuboid
_exptl_crystal_F_000             1084
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.246
_exptl_crystal_size_min          0.124
_refine_diff_density_max         1.099
_refine_diff_density_min         -0.805
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     660
_refine_ls_number_reflns         11633
_refine_ls_number_restraints     107
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0254
_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^)+4.5726P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0568
_refine_ls_wR_factor_ref         0.0591
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10674
_reflns_number_total             11633
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04025k2.cif
_cod_data_source_block           17olg1_0ma
_cod_depositor_comments
'Adding full bibliography for 7701884--7701887.cif.'
_cod_database_code               7701886
_shelx_shelxl_version_number     2018/3
_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. Restrained distances
 C2S-C3S
 1.39 with sigma of 0.05
 C3S-C4S
 1.39 with sigma of 0.05
 C4S-C5S
 1.39 with sigma of 0.05
 C5S-C6S
 1.39 with sigma of 0.05
 C6S-C1S
 1.39 with sigma of 0.05
 C7S-C5S
 1.5 with sigma of 0.02
 C5S-C6S = C1S-C2S = C3S-C4S
 1.4 with sigma of 0.1
 C2T-C3T
 1.39 with sigma of 0.05
 C2T-C1T
 1.39 with sigma of 0.05
 C4T-C6T
 1.39 with sigma of 0.05
 C1T-C7T
 1.39 with sigma of 0.05
 C4T-C7T
 1.39 with sigma of 0.05
 C4T-C5T
 1.5 with sigma of 0.1
3. Restrained planarity
 C4S, C6S, C3S, C7S, C5S, C1S, C2S
 with sigma of 0.1
 C4T, C6T, C3T, C7T, C5T, C1T, C2T
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C4S \\sim C6S \\sim C3S \\sim C7S \\sim C5S \\sim C1S \\sim C2S \\sim C1T \\sim
C3T: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C4T \\sim C2T \\sim C5T \\sim C6T \\sim C7T: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
5. Others
 Sof(C1T)=Sof(H1T)=Sof(C3T)=Sof(H3T)=Sof(C4T)=Sof(C2T)=Sof(H2T)=Sof(C5T)=
 Sof(H5TA)=Sof(H5TB)=Sof(H5TC)=Sof(C6T)=Sof(H6T)=Sof(C7T)=Sof(H7T)=1-FVAR(1)
 Sof(C4S)=Sof(H4S)=Sof(C6S)=Sof(H6S)=Sof(C3S)=Sof(H3S)=Sof(C7S)=Sof(H7SA)=
 Sof(H7SB)=Sof(H7SC)=Sof(C5S)=Sof(C1S)=Sof(H1S)=Sof(C2S)=Sof(H2S)=FVAR(1)
6.a Me refined with riding coordinates:
 C7S(H7SA,H7SB,H7SC), C5T(H5TA,H5TB,H5TC)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C32(H32),
  C33(H33), C34(H34), C35(H35), C36(H36), C42(H42), C43(H43), C44(H44),
 C45(H45), C46(H46), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C62(H62),
  C63(H63), C64(H64), C65(H65), C66(H66), C(H), C8(H8), C10(H10), C17(H17),
 C19(H19), C4S(H4S), C6S(H6S), C3S(H3S), C1S(H1S), C2S(H2S), C1T(H1T), C3T(H3T),
  C2T(H2T), C6T(H6T), C7T(H7T)
6.c Idealised Me refined as rotating group:
 C1B(H1BA,H1BB,H1BC)
;
_shelx_res_checksum              63675
_olex2_submission_special_instructions 'No special instructions were received'