New approach for the synthesis of water soluble fac-[MI(CO)3]+ bis(diarylphosphino)alkylamine complexes (M=99Tc, Re)
Kama, Dumisani Vincent; Frei, Angelo; Brink, Alice; Braband, Henrik; Alberto, Roger; Roodt, Andreas; Dalton Transactions  (2021) –; doi:10.1039/D1DT03234H

data_7708633
_publ_section_title
;
 New approach for the synthesis of water soluble fac-[MI(CO)3]+
 bis(diarylphosphino)alkylamine complexes (M=99Tc, Re)
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03234H
_journal_year                    2021
_chemical_formula_moiety         'C37 H39 Br N O3 P2 Re'
_chemical_formula_sum            'C37 H39 Br N O3 P2 Re'
_chemical_formula_weight         873.74
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-10-12 deposited with the CCDC.	2021-10-20 downloaded from the CCDC.
;
_cell_angle_alpha                92.787(6)
_cell_angle_beta                 111.417(6)
_cell_angle_gamma                104.512(6)
_cell_formula_units_Z            1
_cell_length_a                   9.7040(17)
_cell_length_b                   9.8836(17)
_cell_length_c                   10.5780(19)
_cell_measurement_reflns_used    9853
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.35
_cell_volume                     903.2(3)
_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    'ShelXD (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_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  0.0452
_diffrn_reflns_av_unetI/netI     0.0546
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            15530
_diffrn_reflns_point_group_measured_fraction_full 0.844
_diffrn_reflns_point_group_measured_fraction_max 0.797
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         3.230
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.593
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4892
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.1848 before and 0.0697 after correction.
The Ratio of minimum to maximum transmission is 0.6560.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.606
_exptl_crystal_description       Cuboid
_exptl_crystal_F_000             432
_exptl_crystal_size_max          0.236
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.093
_refine_diff_density_max         1.663
_refine_diff_density_min         -0.737
_refine_diff_density_rms         0.095
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.516(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         6933
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0240
_refine_ls_R_factor_gt           0.0239
_refine_ls_shift/su_max          0.000
_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          0.0515
_refine_ls_wR_factor_ref         0.0515
_reflns_Friedel_coverage         0.598
_reflns_Friedel_fraction_full    0.691
_reflns_Friedel_fraction_max     0.597
_reflns_number_gt                6928
_reflns_number_total             6933
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03234h2.cif
_cod_data_source_block           15dtk1_0m
_cod_database_code               7708633
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.484(7)
 0.516(7)
2. 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
3. Others
 Fixed Sof: Br3(0.15) Br1(0.85)
4.a Ternary CH refined with riding coordinates:
 C1(H1)
4.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B)
4.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C15(H15), C16(H16), C22(H22), C23(H23), C25(H25),
 C26(H26), C32(H32), C33(H33), C35(H35), C36(H36), C42(H42), C43(H43), C45(H45),
  C46(H46)
4.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C27(H27A,H27B,H27C), C37(H37A,H37B,H37C), C47(H47A,H47B,
 H47C)
;
_shelx_res_checksum              86828
_shelx_hkl_checksum              40961
_olex2_submission_special_instructions 'No special instructions were received'