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_7708632
_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         'C32 H35 N P2'
_chemical_formula_sum            'C32 H35 N P2'
_chemical_formula_weight         495.55
_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   mixed
_audit_creation_date             2021-10-05
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-10-05 deposited with the CCDC.	2021-10-20 downloaded from the CCDC.
;
_cell_angle_alpha                64.285(5)
_cell_angle_beta                 81.986(5)
_cell_angle_gamma                68.172(5)
_cell_formula_units_Z            2
_cell_length_a                   11.4833(12)
_cell_length_b                   12.0246(13)
_cell_length_c                   12.2349(13)
_cell_measurement_reflns_used    9830
_cell_measurement_temperature    106(2)
_cell_measurement_theta_max      28.38
_cell_measurement_theta_min      2.69
_cell_volume                     1412.5(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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      106.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0627
_diffrn_reflns_av_unetI/netI     0.0320
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            59293
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.486
_diffrn_reflns_theta_min         2.624
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.174
_exptl_absorpt_correction_T_max  0.7426
_exptl_absorpt_correction_T_min  0.7018
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0869 before and 0.0785 after correction.
The Ratio of minimum to maximum transmission is 0.9451.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.165
_exptl_crystal_description       Cuboid
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.296
_exptl_crystal_size_mid          0.259
_exptl_crystal_size_min          0.118
_refine_diff_density_max         0.309
_refine_diff_density_min         -0.285
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         7095
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0380
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0458P)^2^+0.5522P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0998
_refine_ls_wR_factor_ref         0.1038
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6213
_reflns_number_total             7095
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03234h2.cif
_cod_data_source_block           q1_21dtk5_0m
_cod_database_code               7708632
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.980
_shelx_estimated_absorpt_t_min   0.950
_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.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C4(H4A,H4B), C3(H3A,H3B)
2.b Aromatic/amide H refined with riding coordinates:
 C26(H26), C22(H22), C42(H42), C12(H12), C32(H32), C23(H23), C25(H25),
 C16(H16), C43(H43), C13(H13), C33(H33), C46(H46), C15(H15), C45(H45), C36(H36),
  C35(H35)
2.c Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C47(H47A,H47B,H47C), C37(H37A,H37B,H37C), C17(H17A,H17B,
 H17C)
;
_shelx_res_checksum              19438
_shelx_hkl_checksum              32812
_olex2_submission_special_instructions 'No special instructions were received'