NMR studies of group 8 metallodrugs: <sup>187</sup>Os-enriched organo-osmium half-sandwich anticancer complex.
Needham, Russell J.; Prokes, Ivan; Habtemariam, Abraha; Romero-Canelón, Isolda; Clarkson, Guy J.; Sadler, Peter J.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 12970–12981; doi:10.1039/d1dt02213j

data_7708129
_publ_section_title
;
 NMR studies of group 8 metallodrugs: <sup>187</sup>Os-enriched
 organo-osmium half-sandwich anticancer complex.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12970
_journal_page_last               12981
_journal_paper_doi               10.1039/d1dt02213j
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C23 H28 Br N4 Os, F6 P'
_chemical_formula_sum            'C23 H28 Br F6 N4 Os P'
_chemical_formula_weight         775.57
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2021-02-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-03-01 deposited with the CCDC.	2021-08-09 downloaded from the CCDC.
;
_cell_angle_alpha                85.454(3)
_cell_angle_beta                 79.477(2)
_cell_angle_gamma                82.453(3)
_cell_formula_units_Z            2
_cell_length_a                   8.3437(2)
_cell_length_b                   12.5387(4)
_cell_length_c                   12.6785(3)
_cell_measurement_reflns_used    6763
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.4390
_cell_measurement_theta_min      3.5050
_cell_volume                     1290.73(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2833
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.881
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     37.00  64.00   1.00   10.00    --   14.47 179.00-180.00   27
  2  \w    -11.00  67.00   1.00   10.00    --   14.47  38.00   0.00   78
  3  \w    -63.00  61.00   1.00   10.00    --   14.47 -19.00 150.00  124
  4  \w   -105.00 -77.00   1.00   10.00    --  -15.41-179.00  90.00   28
  5  \w    -95.00 -56.00   1.00   10.00    --  -15.41-179.00 -60.00   39
  6  \w    -22.00  27.00   1.00   10.00    --  -15.41 -99.00  60.00   49
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0617830000
_diffrn_orient_matrix_UB_12      0.0076831000
_diffrn_orient_matrix_UB_13      0.0461501000
_diffrn_orient_matrix_UB_21      -0.0609030000
_diffrn_orient_matrix_UB_22      0.0089213000
_diffrn_orient_matrix_UB_23      -0.0331584000
_diffrn_orient_matrix_UB_31      -0.0075895000
_diffrn_orient_matrix_UB_32      -0.0559293000
_diffrn_orient_matrix_UB_33      0.0043535000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0410
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.881
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12085
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.881
_diffrn_reflns_theta_full        28.000
_diffrn_reflns_theta_max         30.513
_diffrn_reflns_theta_min         3.151
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.613
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.27922
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.996
_exptl_crystal_description       block
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.578
_refine_diff_density_min         -2.552
_refine_diff_density_rms         0.187
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     330
_refine_ls_number_reflns         6943
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0331
_refine_ls_shift/su_max          0.003
_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^+0.4968P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0832
_refine_ls_wR_factor_ref         0.0848
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6634
_reflns_number_total             6943
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 1.9805\% 
 around [0.55 0.84 0.03] (reciprocal) or [0.83 0.55 -0.12] (direct)
;
_cod_data_source_file            d1dt02213j2.cif
_cod_data_source_block           rn3
_cod_depositor_comments          'Adding full bibliography for 7708129.cif.'
_cod_original_cell_volume        1290.73(7)
_cod_database_code               7708129
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C20 H20 N2 F6 P Br Os'
_shelx_estimated_absorpt_t_max   0.458
_shelx_estimated_absorpt_t_min   0.109
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.02
_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
2.a Ternary CH refined with riding coordinates:
 C18(H18), C19(H19), C21(H21), C22(H22), C24(H24)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C10(H10), C11(H11), C13(H13), C14(H14)
2.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C27(H27A,H27B,H27C)
;
_shelx_res_checksum              88369
_shelx_hkl_checksum              82281
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.030
_oxdiff_exptl_absorpt_empirical_full_min 0.570
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2