Coordination-Driven Self-Assembly of Triazole-Based Apoptosis-Inducible Metallomacrocycles.
Singh, Jatinder; Park, Dae Won; Kim, Dong Hwan; Singh, Nem; Kang, Se Chan; Chi, Ki-Whan; ACS omega 4 (2019) 10810–10817; doi:10.1021/acsomega.9b00093

data_4515161
_publ_section_title
;
 Coordination-Driven Self-Assembly of Triazole-Based Apoptosis-Inducible
 Metallomacrocycles.
;
_journal_issue                   6
_journal_name_full               'ACS omega'
_journal_page_first              10810
_journal_page_last               10817
_journal_paper_doi               10.1021/acsomega.9b00093
_journal_volume                  4
_journal_year                    2019
_chemical_formula_moiety         '0.14(C F3 O3 S), 0.03(C132 H108 N16 O8 Ru4)'
_chemical_formula_sum            'C4.61 H3.66 F0.41 N0.54 O0.68 Ru0.14 S0.14'
_chemical_formula_weight         103.28
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-04-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 93.24(3)
_cell_angle_gamma                90
_cell_formula_units_Z            59
_cell_length_a                   15.890(3)
_cell_length_b                   15.537(3)
_cell_length_c                   28.947(6)
_cell_measurement_reflns_used    33327
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      0.980
_cell_measurement_theta_min      0.967
_cell_volume                     7135(2)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.777
_diffrn_measured_fraction_theta_max 0.796
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_unetI/netI     0.0309
_diffrn_reflns_Laue_measured_fraction_full 0.777
_diffrn_reflns_Laue_measured_fraction_max 0.796
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            33238
_diffrn_reflns_point_group_measured_fraction_full 0.777
_diffrn_reflns_point_group_measured_fraction_max 0.796
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.835
_exptl_absorpt_coefficient_mu    0.558
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'clear greenish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3088
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.037
_exptl_transmission_factor_max   0.980
_exptl_transmission_factor_min   0.967
_refine_diff_density_max         1.173
_refine_diff_density_min         -1.170
_refine_diff_density_rms         0.104
_refine_ls_extinction_coef       0.037(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.404
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     872
_refine_ls_number_reflns         10019
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      1.420
_refine_ls_R_factor_all          0.1151
_refine_ls_R_factor_gt           0.1057
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3053
_refine_ls_wR_factor_ref         0.3172
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8022
_reflns_number_total             10019
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao9b00093_si_002.cif
_cod_data_source_block           8
_cod_database_code               4515161
_shelxl_version_number           2013-4
_publ_section_exptl
;
Any special experimental details
;
_shelx_estimated_absorpt_t_max   0.980
_shelx_estimated_absorpt_t_min   0.897
_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. Rigid body (RIGU) restrains
 F3, S1, O7, O6, O5, C88, F1, F2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Ternary CH refined with riding coordinates:
 C49(H49), C67(H67)
3.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C16(H16), C18(H18), C24(H24), C28(H28), C30(H30), C31(H31),
 C33(H33), C35(H35), C37(H37), C39(H39), C41(H41), C42(H42), C43(H43), C44(H44),
  C45(H45), C46(H46), C50(H50), C51(H51), C53(H53), C54(H54), C56(H56),
 C60(H60), C61(H61), C62(H62), C64(H64), C65(H65), C66(H66), C68(H68), C72(H72),
  C73(H73), C75(H75), C77(H77), C80(H80)
3.c Idealised Me refined as rotating group:
 C52(H52A,H52B,H52C), C79(H79A,H79B,H79C), C86(H86A,H86B,H86C), C93(H93A,H93B,
 H93C), C94(H94A,H94B,H94C), C1(H1A,H1B,H1C)
;
_shelx_res_checksum              22254
_shelx_hkl_checksum              46947
_shelx_fab_checksum              72309
_olex2_submission_special_instructions 'No special instructions were received'