A serendipitous crossed aldol reaction in the ligand periphery of a Ru(II) polypyridyl complex in silica bed: prospects for delivering anticancer agents for photoactivated chemotherapy.
Mishra, Ramranjan; Chatterjee, Pritha; Butcher, Ray J.; Patra, Ashis K.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 18484–18493; doi:10.1039/d4dt02337d

data_7717258
_publ_section_title
;
 A serendipitous crossed aldol reaction in the ligand periphery of a
 Ru(II) polypyridyl complex in silica bed: prospects for delivering
 anticancer agents for photoactivated chemotherapy.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              18484
_journal_page_last               18493
_journal_paper_doi               10.1039/d4dt02337d
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety
'2(C49 H38 N8 O2 Ru), 6(N O3), 2(H3 O), H2 O, 4(C2 H3 N)'
_chemical_formula_sum            'C106 H96 N26 O25 Ru2'
_chemical_formula_weight         2336.22
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-07-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-08-16 deposited with the CCDC.	2024-10-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.404(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.809(3)
_cell_length_b                   20.790(6)
_cell_length_c                   21.430(6)
_cell_measurement_reflns_used    9804
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.17
_cell_measurement_theta_min      2.53
_cell_volume                     5138(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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0930
_diffrn_reflns_av_unetI/netI     0.0535
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            105756
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.406
_diffrn_reflns_theta_min         2.330
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.385
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6946
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'metallic dark red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_description       block
_exptl_crystal_F_000             2404
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.384
_refine_diff_density_min         -0.850
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     810
_refine_ls_number_reflns         12796
_refine_ls_number_restraints     177
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0925
_refine_ls_R_factor_gt           0.0682
_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^)+(0.0512P)^2^+20.8555P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1510
_refine_ls_wR_factor_ref         0.1635
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9920
_reflns_number_total             12796
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02337d2.cif
_cod_data_source_block           '[1-Ac]'
_cod_depositor_comments          'Adding full bibliography for 7717258.cif.'
_cod_database_code               7717258
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.955
_shelx_estimated_absorpt_t_min   0.910
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups, All O(H,H,H) groups
2. Restrained distances
 O1W-H1WA = O1W-H1WB = O1W-H1WC
 0.82 with sigma of 0.02
 H1WA-H1WB = H1WA-H1WC = H1WB-H1WC
 1.339 with sigma of 0.02
 O2W-H2WA = O2W-H2WB
 0.82 with sigma of 0.02
 H2WA-H2WB
 1.297 with sigma of 0.02
3. Rigid bond restraints
 O1A, O1B
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 N12, C50, C51, N12A, C50A, C51A
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 N13, C52, C53, N13A, C52A, C53A
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
O1A \\sim O1B: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01
N12 \\sim C50 \\sim C51 \\sim N12A \\sim C50A \\sim C51A: within 2A with sigma
of 0.005 and sigma for terminal atoms of 0.01
N13 \\sim C52 \\sim C53 \\sim N13A \\sim C52A \\sim C53A: within 2A with sigma
of 0.005 and sigma for terminal atoms of 0.01
5. Same fragment restrains
{N12, C50, C51} sigma for 1-2: 0.005, 1-3: 0.04
as
{N12A, C50A, C51A}
{N12, C50, C51} sigma for 1-2: 0.005, 1-3: 0.04
as
{N13, C52, C53}
{N12, C50, C51} sigma for 1-2: 0.005, 1-3: 0.04
as
{N13A, C52A, C53A}
6. Others
 Sof(O1B)=Sof(H1B)=Sof(H44A)=1-FVAR(1)
 Sof(O1A)=Sof(H1A)=Sof(H44)=FVAR(1)
 Sof(N12A)=Sof(C50A)=Sof(C51A)=Sof(H51D)=Sof(H51E)=Sof(H51F)=1-FVAR(2)
 Sof(N12)=Sof(C50)=Sof(C51)=Sof(H51A)=Sof(H51B)=Sof(H51C)=FVAR(2)
 Sof(N13A)=Sof(C52A)=Sof(C53A)=Sof(H53D)=Sof(H53E)=Sof(H53F)=1-FVAR(3)
 Sof(N13)=Sof(C52)=Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(H53C)=FVAR(3)
 Fixed Sof: O2W(0.5) H2WA(0.5) H2WB(0.5)
7.a Ternary CH refined with riding coordinates:
 C44(H44), C44(H44A)
7.b Secondary CH2 refined with riding coordinates:
 C45(H45A,H45B)
7.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C10(H10), C11(H11), C14(H14),
 C15(H15), C16(H16), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24),
  C25(H25), C29(H29), C30(H30), C31(H31), C32(H32), C36(H36), C37(H37),
 C38(H38), C41(H41), C42(H42), C48(H48), C49(H49)
7.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C47(H47A,H47B,H47C), C51(H51A,H51B,H51C), C51A(H51D,H51E,
 H51F), C53(H53A,H53B,H53C), C53A(H53D,H53E,H53F)
7.e Idealised tetrahedral OH refined as rotating group:
 O1A(H1A), O1B(H1B)
;
_shelx_res_checksum              97980
_shelx_hkl_checksum              23289
_olex2_submission_special_instructions 'No special instructions were received'