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_7701884
_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         'C14 H7 N O8 Re, C14 H8 N O8 Re, 2(H2 O)'
_chemical_formula_sum            'C28 H19 N2 O18 Re2'
_chemical_formula_weight         1043.85
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-08-15
_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                90
_cell_angle_beta                 100.373(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.848(2)
_cell_length_b                   11.667(3)
_cell_length_c                   19.101(3)
_cell_measurement_reflns_used    9440
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.46
_cell_measurement_theta_min      3.17
_cell_volume                     6104.5(19)
_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)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_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  0.0470
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            55766
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         27.997
_diffrn_reflns_theta_min         1.487
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.015
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5615
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0918 before and 0.0593 after correction.
The Ratio of minimum to maximum transmission is 0.7530.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.272
_exptl_crystal_description       Cuboid
_exptl_crystal_F_000             3960
_exptl_crystal_size_max          0.526
_exptl_crystal_size_mid          0.237
_exptl_crystal_size_min          0.069
_refine_diff_density_max         1.447
_refine_diff_density_min         -0.990
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         7356
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_gt           0.0220
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0295P)^2^+21.9010P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0565
_refine_ls_wR_factor_ref         0.0592
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6594
_reflns_number_total             7356
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04025k2.cif
_cod_data_source_block           16dlg2_0ma
_cod_depositor_comments
'Adding full bibliography for 7701884--7701887.cif.'
_cod_database_code               7701884
_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 O(H) groups, All O(H,H) groups
2.a Free rotating group:
 O10(H10A,H10B), O1(H1A,H1B)
2.b Rotating group:
 O08A(H08E,H08F), O08B(H08A,H08C)
2.c Aromatic/amide H refined with riding coordinates:
 C05A(H05A), C05B(H05B), C06A(H06C), C06B(H06B), C07A(H07A), C07B(H07B),
 C08A(H08D), C08B(H08B), C12A(H12A), C12B(H12B)
2.d Idealised tetrahedral OH refined as rotating group:
 O06B(H06A)
;
_shelx_res_checksum              55058
_olex2_submission_special_instructions 'No special instructions were received'