Increasing anti-cancer activity with longer tether lengths of group 9 Cp* complexes.
Lucas, Stephanie J.; Lord, Rianne M.; Basri, Aida M.; Allison, Simon J.; Phillips, Roger M.; Blacker, A. John; McGowan, Patrick C.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 6812–6815; doi:10.1039/c6dt00186f

data_7038418
_publ_section_title
;
 Increasing anti-cancer activity with longer tether lengths of group 9 Cp*
 complexes.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6812
_journal_page_last               6815
_journal_paper_doi               10.1039/c6dt00186f
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C26 H31 Cl2 Ir N2 O2, C H2 Cl2'
_chemical_formula_sum            'C27 H33 Cl4 Ir N2 O2'
_chemical_formula_weight         751.55
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-12-02
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2015-12-11 deposited with the CCDC.
2016-02-17 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 93.344(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.353(3)
_cell_length_b                   16.197(2)
_cell_length_c                   14.631(2)
_cell_measurement_reflns_used    7989
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.415
_cell_measurement_theta_min      2.46
_cell_volume                     5761.3(13)
_computing_cell_refinement       'APEX 2 software, Bruker Nonius 2004'
_computing_data_collection       'APEX 2 software, Bruker Nonius 2004'
_computing_data_reduction        'SAINT, Bruker Nonius 2004'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL-1997 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean '120 microns'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker X8 Apex diffractometer'
_diffrn_measurement_method       'Rotation images'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0538
_diffrn_reflns_av_unetI/netI     0.0193
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            285232
_diffrn_reflns_theta_full        30.42
_diffrn_reflns_theta_max         30.42
_diffrn_reflns_theta_min         2.02
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.033
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4288
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1174 before and 0.0639 after correction.
The Ratio of minimum to maximum transmission is 0.5747.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.733
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2960
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.602
_refine_diff_density_min         -1.485
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     671
_refine_ls_number_reflns         17410
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0257
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0255P)^2^+14.3636P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0605
_refine_ls_wR_factor_ref         0.0688
_reflns_number_gt                14621
_reflns_number_total             17410
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt00186f2.cif
_cod_data_source_block           sjl196
_cod_depositor_comments
'Adding full bibliography for 7038415--7038419.cif.'
_cod_original_cell_volume        5761.3(14)
_cod_database_code               7038418
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl4B-C15B
 1.74 with sigma of 0.01
 Cl3B-C15B
 1.74 with sigma of 0.01
 Cl4-C15 = Cl3-C15
 1.74 with sigma of 0.01
3. Others
 Fixed Sof: Cl3(0.87) Cl4(0.87) C15(0.87) H15A(0.87) H15B(0.87) Cl4B(0.13)
 Cl3B(0.13) C15B(0.13) H15E(0.13) H15F(0.13)
4.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C10A(H10C,H10D), C11(H11A,H11B), C11A(H11C,H11D), C12(H12A,
 H12B), C12A(H12C,H12D), C13(H13A,H13B), C13A(H13C,H13D), C14(H14A,H14B),
 C14A(H14C,H14D), C15(H15A,H15B), C15A(H15C,H15D), C15B(H15E,H15F)
4.b Aromatic/amide H refined with riding coordinates:
 C31(H31), C31A(H31A), C32(H32), C32A(H32A), C33(H33), C33A(H33A), C34(H34),
 C34A(H34A), C38(H38), C38A(H38A), C40(H40), C40A(H40A), C41(H41), C41A(H41A),
 C42(H42), C42A(H42A)
4.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C6A(H6AA,H6AB,H6AC), C7(H7A,H7B,H7C), C7A(H7AA,H7AB,H7AC),
 C8(H8A,H8B,H8C), C8A(H8AA,H8AB,H8AC), C9(H9A,H9B,H9C), C9A(H9AA,H9AB,H9AC)
4.d Idealised tetrahedral OH refined as rotating group:
 O1(H1), O1A(H1A)
;
_olex2_submission_special_instructions 'No special instructions were received'