Ruthenium bistridentate complexes with non-symmetrical hexahydro-pyrimidopyrimidine ligands: a structural and theoretical investigation of their optical and electrochemical properties.
Laramée-Milette, Baptiste; Hanan, Garry S.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 12507–12517; doi:10.1039/c6dt02408d

data_7039902
_publ_section_title
;
 Ruthenium bistridentate complexes with non-symmetrical
 hexahydro-pyrimidopyrimidine ligands: a structural and theoretical
 investigation of their optical and electrochemical properties.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12507
_journal_page_last               12517
_journal_paper_doi               10.1039/c6dt02408d
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C42 H42 N10 Ru, 2(F6 P), C2 H3 N'
_chemical_formula_sum            'C44 H45 F12 N11 P2 Ru'
_chemical_formula_weight         1118.92
_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
_audit_creation_date             2016-04-01
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-04-04 deposited with the CCDC.
2016-07-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.456(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.1907(6)
_cell_length_b                   8.1133(2)
_cell_length_c                   24.9115(6)
_cell_measurement_reflns_used    9960
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.12
_cell_measurement_theta_min      3.66
_cell_volume                     4343.06(19)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1017
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            105462
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.590
_diffrn_reflns_theta_min         2.056
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.524
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.5771
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.1119 before and 0.0745 after correction.
The Ratio of minimum to maximum transmission is 0.7658.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.711
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2272
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.559
_refine_diff_density_min         -0.586
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     632
_refine_ls_number_reflns         8562
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0770
_refine_ls_R_factor_gt           0.0621
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0790P)^2^+13.2320P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1554
_refine_ls_wR_factor_ref         0.1659
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6926
_reflns_number_total             8562
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02408d2.cif
_cod_data_source_block           bala71_0m
_cod_depositor_comments
'Adding full bibliography for 7039900--7039902.cif.'
_cod_database_code               7039902
_shelx_estimated_absorpt_t_max   144.245
_shelx_estimated_absorpt_t_min   7.329
_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
2.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C39(H39A,H39B), C40(H40A,H40B), C38(H38A,H38B), C41(H41A,
 H41B), C17(H17A,H17B), C36(H36A,H36B), C37(H37A,H37B), C16(H16A,H16B),
 C18(H18A,H18B), C15(H15A,H15B), C19(H19A,H19B)
2.b Aromatic/amide H refined with riding coordinates:
 C32(H32), C4(H4), C13(H13), C12(H12), C29(H29), C11(H11), C3(H3), C2(H2),
 C23(H23), C34(H34), C6(H6), C8(H8), C25(H25), C24(H24), C33(H33), C28(H28),
 C7(H7), C27(H27)
2.c Idealised Me refined as rotating group:
 C01Y(H01A,H01B,H01C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'