New activation mechanism for half-sandwich organometallic anticancer complexes.
Banerjee, Samya; Soldevila-Barreda, Joan J; Wolny, Juliusz A.; Wootton, Christopher A.; Habtemariam, Abraha; Romero-Canelón, Isolda; Chen, Feng; Clarkson, Guy J.; Prokes, Ivan; Song, Lijiang; O'Connor, Peter B; Schünemann, Volker; Sadler, Peter J.; Chemical science 9 (2018) 3177–3185; doi:10.1039/c7sc05058e

data_1549017
_publ_section_title
;
 New activation mechanism for half-sandwich organometallic anticancer
 complexes.
;
_journal_issue                   12
_journal_name_full               'Chemical science'
_journal_page_first              3177
_journal_page_last               3185
_journal_paper_doi               10.1039/c7sc05058e
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety         'C31 H29 Cl N2 Rh, C3 H6 O, F6 P'
_chemical_formula_sum            'C34 H35 Cl F6 N2 O P Rh'
_chemical_formula_weight         770.97
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_block_doi                 10.5517/ccdc.csd.cc1jnp40
_audit_creation_date             2015-04-28
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-08-22 deposited with the CCDC.
2018-02-19 downloaded from the CCDC.
;
_cell_angle_alpha                80.000(2)
_cell_angle_beta                 86.442(2)
_cell_angle_gamma                86.175(2)
_cell_formula_units_Z            2
_cell_length_a                   8.40215(19)
_cell_length_b                   12.9603(3)
_cell_length_c                   15.3920(4)
_cell_measurement_reflns_used    11352
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      78.3330
_cell_measurement_theta_min      4.1290
_cell_volume                     1644.79(7)
_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
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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, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1417
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_details
;
  1 omega  -18.00   33.00   1.0000    6.5000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   36.0000   74.0000 51

  2 omega  -90.00   -1.00   1.0000    6.5000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  125.0000  -60.0000 89

  3 omega  -50.00    1.00   1.0000    6.5000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000  -30.0000 51

  4 omega -105.00  -33.00   1.0000    6.5000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -38.0000   90.0000 72

  5 omega -107.00  -13.00   1.0000    6.5000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -57.0000 -180.0000 94

  6 omega   54.00   88.00   1.0000    6.5000
omega____ theta____ kappa____ phi______ frames
    -       42.8790 -125.0000 -180.0000 34

  7 omega  107.00  178.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000   45.0000 -120.0000 71

  8 omega   92.00  174.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000   45.0000  -60.0000 82

  9 omega   46.00  121.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000  -61.0000  -90.0000 75

 10 omega   63.00   91.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000  -30.0000    0.0000 28

 11 omega   42.00   87.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000  -30.0000  -90.0000 45

 12 omega   63.00  116.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000 -111.0000  -60.0000 53

 13 omega   35.00   85.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000  -95.0000 -180.0000 50

 14 omega   44.00   91.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000  -30.0000  120.0000 47

 15 omega   80.00  112.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000 -111.0000   30.0000 32

 16 omega  124.00  151.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000   30.0000   30.0000 27

 17 omega   42.00  114.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000 -111.0000 -180.0000 72

 18 omega  101.00  137.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000  -61.0000  150.0000 36

 19 omega   57.00  104.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000  -95.0000   90.0000 47

 20 omega   83.00  116.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000 -111.0000   90.0000 33

 21 omega  114.00  177.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000   30.0000    0.0000 63

 22 omega   44.00   87.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000  -45.0000 -180.0000 43

 23 omega   36.00   85.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000  -95.0000   30.0000 49

 24 omega   62.00  114.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000 -111.0000 -120.0000 52

 25 omega   84.00  113.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000 -111.0000  -30.0000 29

 26 omega  101.00  171.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000  111.0000 -180.0000 70

 27 omega  118.00  178.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000  111.0000 -120.0000 60

 28 omega  -50.00   33.00   1.0000    6.5000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000  150.0000 83

 29 omega   18.00  111.00   1.0000    6.5000
omega____ theta____ kappa____ phi______ frames
    -       42.8790   57.0000   90.0000 93

 30 omega   13.00  112.00   1.0000    6.5000
omega____ theta____ kappa____ phi______ frames
    -       42.8790   77.0000 -150.0000 99

 31 omega   13.00  114.00   1.0000    6.5000
omega____ theta____ kappa____ phi______ frames
    -       42.8790   77.0000  -30.0000 101
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0085430000
_diffrn_orient_matrix_UB_12      0.1154883000
_diffrn_orient_matrix_UB_13      -0.0461888000
_diffrn_orient_matrix_UB_21      -0.1836148000
_diffrn_orient_matrix_UB_22      -0.0001151000
_diffrn_orient_matrix_UB_23      0.0032398000
_diffrn_orient_matrix_UB_31      -0.0084055000
_diffrn_orient_matrix_UB_32      0.0357579000
_diffrn_orient_matrix_UB_33      0.0906236000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_unetI/netI     0.0399
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            18378
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.769
_diffrn_reflns_theta_min         4.137
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.975
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42379
_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.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_description       block
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.789
_refine_diff_density_min         -1.004
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         6984
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.431
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0332
_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^)+(0.0523P)^2^+0.9670P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0883
_refine_ls_wR_factor_ref         0.0897
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6552
_reflns_number_total             6984
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc05058e2.cif
_cod_data_source_block           js18
_cod_depositor_comments
'Adding full bibliography for 1549011--1549018.cif.'
_cod_original_cell_volume        1644.78(7)
_cod_database_code               1549017
_chemical_oxdiff_formula         'C20 H20 N2 O2 F6 P Cl Rh'
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     75.12
_olex2_refinement_description
;
A SIMU restraint was used to give two fluorides in the PF6 
reasonably similar thermal parameters.

1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
P10 \\sim F14 \\sim F13: within 1.7A with sigma of 0.0008 and sigma for
terminal atoms of 0.0016
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11), C13(H13),
 C14(H14), C15(H15), C16(H16), C17(H17), C20(H20), C21(H21), C23(H23), C24(H24)
3.b Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,
 H33C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'