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_7039900
_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         'C34 H38 N10 Ru, 2(F6 P), C4 H6 O'
_chemical_formula_sum            'C38 H44 F12 N10 O P2 Ru'
_chemical_formula_weight         1047.84
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 99.4770(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3080(4)
_cell_length_b                   26.7172(8)
_cell_length_c                   14.0045(5)
_cell_measurement_reflns_used    9868
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      59.87
_cell_measurement_theta_min      4.31
_cell_volume                     4173.3(2)
_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 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_unetI/netI     0.0158
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            47209
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         59.841
_diffrn_reflns_theta_min         2.878
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.042
_exptl_absorpt_correction_T_max  0.7517
_exptl_absorpt_correction_T_min  0.5457
_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            purple
_exptl_crystal_density_diffrn    1.668
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.967
_refine_diff_density_min         -0.803
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4674
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0354
_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^)+(0.0530P)^2^+12.0210P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0944
_refine_ls_wR_factor_ref         0.0947
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4598
_reflns_number_total             4674
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02408d2.cif
_cod_data_source_block           bala65_0m
_cod_depositor_comments
'Adding full bibliography for 7039900--7039902.cif.'
_cod_database_code               7039900
_shelx_estimated_absorpt_t_max   119.748
_shelx_estimated_absorpt_t_min   8.617
_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. Restrained distances
 C19_$1-C18_$1
 1.54 with sigma of 0.02
 C18-C19
 1.54 with sigma of 0.02
 C19_$1-O1_$1
 1.43 with sigma of 0.02
 C19-O1_$1
 1.43 with sigma of 0.02
 C18_$1-O1_$1
 2.36 with sigma of 0.04
 C18-O1_$1
 2.36 with sigma of 0.04
 C19_$1-C19
 2.35 with sigma of 0.04
3. Rigid bond restraints
 O1, C19, C18
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C18
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O1 \\sim C19 \\sim C18: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C18 \\sim C19: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
5. Others
 Fixed Sof: O1(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C16(H16A,H16B), C14(H14A,H14B), C11(H11A,H11B), C12(H12A,
 H12B), C15(H15A,H15B)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C7(H7), C2(H2), C3(H3), C4(H4), C9(H9), C8(H8)
6.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'