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_7708634
_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 Cl N O3 P2 Tc'
_chemical_formula_sum            'C37 H39 Cl N O3 P2 Tc'
_chemical_formula_weight         741.08
_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
_audit_creation_date             2021-10-12
_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                92.434(3)
_cell_angle_beta                 111.683(3)
_cell_angle_gamma                104.288(3)
_cell_formula_units_Z            1
_cell_length_a                   9.6184(3)
_cell_length_b                   9.8959(4)
_cell_length_c                   10.6919(4)
_cell_measurement_reflns_used    6867
_cell_measurement_temperature    182.9(6)
_cell_measurement_theta_max      29.0160
_cell_measurement_theta_min      3.0180
_cell_volume                     906.27(6)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01)'
_computing_data_collection
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01)'
_computing_data_reduction
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      182.9(6)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4498
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
'#__ type_ start__ end____ width___ exp.time_ 1 omega 10.00 64.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 16.1514 57.0000 -90.0000 54 #__ type_ start__ end____ width___ exp.time_ 2 omega 13.00 89.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 16.1514 57.0000 -30.0000 76 #__ type_ start__ end____ width___ exp.time_ 3 omega 1.00 63.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 16.1514 57.0000 -150.0000 62 #__ type_ start__ end____ width___ exp.time_ 4 omega -25.00 23.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 16.1514 -48.0000 -19.0000 48 #__ type_ start__ end____ width___ exp.time_ 5 omega -12.00 89.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 16.1514 60.0000 104.2145 101 #__ type_ start__ end____ width___ exp.time_ 6 omega 53.00 79.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 16.1514 38.0000 30.0000 26 #__ type_ start__ end____ width___ exp.time_ 7 omega -38.00 48.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 18.0000 -58.0000 52.5966 86 #__ type_ start__ end____ width___ exp.time_ 8 omega -39.00 48.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 18.0000 -59.0000 -138.5858 87 #__ type_ start__ end____ width___ exp.time_ 9 omega -54.00 45.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 18.0000 -57.0000 -34.2645 99 #__ type_ start__ end____ width___ exp.time_ 10 omega -28.00 9.00 1.0000 90.0000 omega____ theta____ kappa____ phi______ frames - 18.0000 -60.0000 143.0809 37'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0253209000
_diffrn_orient_matrix_UB_12      -0.0631475000
_diffrn_orient_matrix_UB_13      0.0243561000
_diffrn_orient_matrix_UB_21      -0.0343061000
_diffrn_orient_matrix_UB_22      0.0352275000
_diffrn_orient_matrix_UB_23      0.0346041000
_diffrn_orient_matrix_UB_31      -0.0709241000
_diffrn_orient_matrix_UB_32      -0.0191637000
_diffrn_orient_matrix_UB_33      -0.0585064000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_av_unetI/netI     0.0651
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15248
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         3.021
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.594
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71362
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_description       cube
_exptl_crystal_F_000             382
_exptl_crystal_size_max          0.222
_exptl_crystal_size_mid          0.119
_exptl_crystal_size_min          0.099
_refine_diff_density_max         1.044
_refine_diff_density_min         -0.879
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.38(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         8390
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0459
_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^)+(0.0522P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0992
_refine_ls_wR_factor_ref         0.1035
_reflns_Friedel_coverage         0.922
_reflns_Friedel_fraction_full    0.948
_reflns_Friedel_fraction_max     0.920
_reflns_number_gt                7693
_reflns_number_total             8390
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03234h2.cif
_cod_data_source_block           tdk150615
_cod_database_code               7708634
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.944
_shelx_estimated_absorpt_t_min   0.879
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.62(4)
 0.38(4)
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. Uiso/Uaniso restraints and constraints
Uanis(C6) = Uanis(C3)
Uanis(C1) = Uanis(C4)
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              6434
_shelx_hkl_checksum              43809
_olex2_submission_special_instructions 'No special instructions were received'