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_1549018
_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         'C27 H25 Cl N2 Rh, 2(F3 P0.5), C H4 O'
_chemical_formula_sum            'C28 H29 Cl F6 N2 O P Rh'
_chemical_formula_weight         692.86
_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   mixed
_atom_sites_solution_primary     direct
_audit_block_doi                 10.5517/ccdc.csd.cc1jnp3z
_audit_creation_date             2014-12-05
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.28 svn.r3107 for OlexSys, GUI svn.r4959)
;
_audit_update_record
;
2015-08-22 deposited with the CCDC.
2018-02-19 downloaded from the CCDC.
;
_cell_angle_alpha                82.3397(11)
_cell_angle_beta                 81.4575(11)
_cell_angle_gamma                84.0175(9)
_cell_formula_units_Z            2
_cell_length_a                   8.20707(8)
_cell_length_b                   10.08952(12)
_cell_length_c                   17.2032(3)
_cell_measurement_reflns_used    41298
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.0630
_cell_measurement_theta_min      2.5200
_cell_volume                     1390.95(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2833
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_details
;
  1 omega  -11.00   90.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       17.2579   57.0000    0.0000 101

  2 omega  -25.00   58.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       17.2579  -99.0000 -150.0000 83

  3 omega  -24.00   97.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       17.2579   19.0000  150.0000 121

  4 omega  -57.00   42.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       17.2579  -38.0000  -30.0000 99

  5 omega  -25.00   58.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       17.2579  -99.0000  120.0000 83

  6 omega  -15.00   93.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       17.2579   77.0000 -120.0000 108

  7 omega  -84.00  -29.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.1954  141.0000  -65.0000 55

  8 omega  -25.00   23.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.1954  -99.0000  120.0000 48

  9 omega  -90.00  -33.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.1954  149.0000 -168.2064 57

 10 omega  -11.00   90.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       17.2579   57.0000   90.0000 101

 11 omega   35.00  106.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       17.2579  178.0000 -120.0000 71

 12 omega   35.00  106.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       17.2579  178.0000    0.0000 71

 13 omega  -77.00  -22.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.1954  129.0000  122.0000 55

 14 omega  -88.00  -32.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.1954  147.0000 -151.9336 56

 15 omega  -75.00  -19.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.1954  126.0000   34.1273 56

 16 omega  -25.00   23.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.1954  -99.0000   30.0000 48

 17 omega  -71.00   91.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       17.2579    0.0000 -120.0000 162

 18 omega  -71.00  105.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       17.2579    0.0000 -180.0000 176

 19 omega  -71.00  105.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       17.2579    0.0000 -150.0000 176

 20 omega -106.00   70.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.1954    0.0000 -180.0000 176

 21 omega  -77.00  -22.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.1954  129.0000   17.4126 55
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0305874000
_diffrn_orient_matrix_UB_12      0.0686191000
_diffrn_orient_matrix_UB_13      -0.0029616000
_diffrn_orient_matrix_UB_21      0.0105589000
_diffrn_orient_matrix_UB_22      0.0028667000
_diffrn_orient_matrix_UB_23      -0.0418495000
_diffrn_orient_matrix_UB_31      -0.0815347000
_diffrn_orient_matrix_UB_32      -0.0187726000
_diffrn_orient_matrix_UB_33      0.0018636000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            86143
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.376
_diffrn_reflns_theta_min         2.412
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.834
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90601
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
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    1.654
_exptl_crystal_description       block
_exptl_crystal_F_000             700
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.598
_refine_diff_density_min         -0.488
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         9499
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0281
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0294P)^2^+0.8061P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0642
_refine_ls_wR_factor_ref         0.0681
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8447
_reflns_number_total             9499
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc05058e2.cif
_cod_data_source_block           js17
_cod_depositor_comments
'Adding full bibliography for 1549011--1549018.cif.'
_cod_original_cell_volume        1390.96(3)
_cod_database_code               1549018
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C20 H20 N2 O2 F6 P Rh'
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All F(H) groups
2. Others
 Fixed Sof: F22(0.55) F23(0.55) F23A(0.3) F22A(0.3) F22B(0.15) F23B(0.15)
3.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C10(H10), C9(H9), C11(H11), C6(H6), C2(H2), C4(H4), C19(H19),
 C18(H18), C16(H16), C3(H3), C15(H15), C17(H17)
3.b Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C26(H26A,H26B,H26C), C28(H28A,H28B,
 H28C), C31(H31A,H31B,H31C)
;
_olex2_submission_special_instructions 'No special instructions were received'