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_7039901
_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         'C38 H34 N8 Ru, 2(F6 P), C3 H6 O'
_chemical_formula_sum            'C41 H40 F12 N8 O P2 Ru'
_chemical_formula_weight         1051.82
_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   geom
_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                69.3920(10)
_cell_angle_beta                 80.4920(10)
_cell_angle_gamma                79.5240(10)
_cell_formula_units_Z            4
_cell_length_a                   13.4632(3)
_cell_length_b                   17.4582(5)
_cell_length_c                   19.4702(5)
_cell_measurement_reflns_used    8978
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      53.94
_cell_measurement_theta_min      2.61
_cell_volume                     4186.57(19)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3418
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            18299
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        53.618
_diffrn_reflns_theta_max         59.876
_diffrn_reflns_theta_min         2.123
_exptl_absorpt_coefficient_mu    3.066
_exptl_absorpt_correction_T_max  0.7517
_exptl_absorpt_correction_T_min  0.5773
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.1302 before and 0.0454 after correction.
The Ratio of minimum to maximum transmission is 0.7260.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.669
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.176
_refine_diff_density_min         -0.669
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1179
_refine_ls_number_reflns         18299
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0331
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0450P)^2^+4.1787P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0835
_refine_ls_wR_factor_ref         0.0857
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17364
_reflns_number_total             18299
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02408d2.cif
_cod_data_source_block           bala66_0m
_cod_depositor_comments
;
Adding full bibliography for 7039900--7039902.cif.

2018-06-07
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '4(C38 H34 N8 Ru), 8(F6 P), 4(C3 H6 O)'
_cod_original_formula_sum        'C164 H160 F48 N32 O4 P8 Ru4'
_cod_original_formula_units_Z    1
_cod_original_formula_weight     4207.27
_cod_database_code               7039901
_shelx_estimated_absorpt_t_max   119.709
_shelx_estimated_absorpt_t_min   4.749
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.6209(5) 0.3791(5)
2. 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
3.a Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C74(H74A,H74B), C34(H34A,H34B), C37(H37A,H37B), C71(H71A,
 H71B), C38(H38A,H38B), C36(H36A,H36B), C72(H72A,H72B), C33(H33A,H33B),
 C70(H70A,H70B), C76(H76A,H76B), C75(H75A,H75B)
3.b Aromatic/amide H refined with riding coordinates:
 C60(H60), C15(H15), C7(H7), C22(H22), C61(H61), C53(H53), C12(H12), C63(H63),
 C68(H68), C42(H42), C25(H25), C45(H45), C47(H47), C14(H14), C39(H39), C41(H41),
  C13(H13), C4(H4), C3(H3), C50(H50), C9(H9), C67(H67), C30(H30), C23(H23),
 C2(H2), C56(H56), C40(H40), C52(H52), C55(H55), C66(H66), C28(H28), C20(H20),
 C24(H24), C62(H62), C1(H1), C21(H21), C29(H29), C51(H51), C59(H59), C18(H18),
 C57(H57), C58(H58), C19(H19), C17(H17)
3.c Idealised Me refined as rotating group:
 C82(H82A,H82B,H82C), C79(H79A,H79B,H79C), C80(H80A,H80B,H80C), C77(H77A,H77B,
 H77C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'