An investigation on 3-acetyl-7-methoxy-coumarin Schiff bases and their Ru(ii) metallates with potent antiproliferative activity and enhanced LDH and NO release
Kalaiarasi, G.; Jeya Rajkumar, S. Rex; Dharani, S.; Małecki, J. G.; Prabhakaran, R.; RSC Advances 8 (2018) 1539–; doi:10.1039/C7RA12104K

data_7229880
_publ_section_title
;
 An investigation on 3-acetyl-7-methoxy-coumarin Schiff bases and their
 Ru(ii) metallates with potent antiproliferative activity and enhanced LDH
 and NO release
;
_journal_issue                   3
_journal_name_full               'RSC Advances'
_journal_page_first              1539
_journal_paper_doi               10.1039/C7RA12104K
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety         'C50 H41 N3 O4 P2 Ru S, C H4 O'
_chemical_formula_sum            'C51 H45 N3 O5 P2 Ru S'
_chemical_formula_weight         974.97
_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   mixed
_atom_sites_solution_primary     heavy
_audit_creation_date             2017-05-25
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2017-10-16 deposited with the CCDC.
2017-12-18 downloaded from the CCDC.
;
_cell_angle_alpha                89.094(3)
_cell_angle_beta                 75.301(3)
_cell_angle_gamma                70.576(3)
_cell_formula_units_Z            2
_cell_length_a                   13.0569(5)
_cell_length_b                   13.7232(5)
_cell_length_c                   13.8479(5)
_cell_measurement_reflns_used    8480
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.9990
_cell_measurement_theta_min      3.7930
_cell_volume                     2257.08(16)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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      295(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4015
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.846
_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    -33.00  56.00   1.00   54.52    --  -11.62  57.00  30.00   89
  2  \w     -6.00  25.00   1.00   54.52    --    9.75  19.00 -90.00   31
  3  \w    -35.00  63.00   1.00   54.52    --  -11.62  77.00  90.00   98
  4  \w    -82.00  17.00   1.00   54.52    --  -11.62 -57.00-120.00   99
  5  \w    -68.00 -35.00   1.00   54.52    --    9.75-179.00  30.00   33
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0114431000
_diffrn_orient_matrix_UB_12      0.0522518000
_diffrn_orient_matrix_UB_13      0.0161006000
_diffrn_orient_matrix_UB_21      0.0445366000
_diffrn_orient_matrix_UB_22      -0.0161821000
_diffrn_orient_matrix_UB_23      0.0236442000
_diffrn_orient_matrix_UB_31      0.0380939000
_diffrn_orient_matrix_UB_32      0.0053482000
_diffrn_orient_matrix_UB_33      -0.0447410000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_av_unetI/netI     0.0584
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.846
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            21925
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.846
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.501
_diffrn_reflns_theta_min         3.302
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.516
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82670
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_description       plate
_exptl_crystal_F_000             1004
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.933
_refine_diff_density_min         -0.588
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     580
_refine_ls_number_reflns         10636
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0390
_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^)+(0.0400P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0833
_refine_ls_wR_factor_ref         0.0924
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8354
_reflns_number_total             10636
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra12104k2.cif
_cod_data_source_block           ruh7a2
_cod_original_cell_volume        2257.10(15)
_cod_database_code               7229880
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         'Ru1 P2 O4 N3 S1 C50 H45'
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C10(H10), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20),
 C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C28(H28), C29(H29), C30(H30),
  C31(H31), C32(H32), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38),
 C40(H40), C41(H41), C42(H42), C43(H43), C44(H44), C46(H46), C47(H47), C48(H48),
  C49(H49), C50(H50)
2.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C51(H51A,H51B,H51C)
2.c Idealised tetrahedral OH refined as rotating group:
 O5(H5)
;
_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 1.268
_oxdiff_exptl_absorpt_empirical_full_min 0.830