Three Steps in One Pot: Synthesis of Linear Bilateral Extended 2,2':6',2″-Terpyridineruthenium(II) Complexes.
Veliks, Janis; Blacque, Olivier; Siegel, Jay S.; Inorganic chemistry  (2014) 141028140700007–; doi:10.1021/ic501946f

data_4341408
_publ_section_title
;
 Three Steps in One Pot: Synthesis of Linear Bilateral Extended
 2,2':6',2&#x2033;-Terpyridineruthenium(II) Complexes.
;
_journal_name_full               'Inorganic chemistry'
_journal_page_first              141028140700007
_journal_paper_doi               10.1021/ic501946f
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety
' C70 H50 Br4 N6 O4 Ru, 2(F6 P), 2(C4 H10 O), 2(C2 H3 N)'
_chemical_formula_sum            'C82 H76 Br4 F12 N8 O6 P2 Ru'
_chemical_formula_weight         1980.15
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-02-24
_audit_creation_method
;
Olex2 1.2
(compiled 2014.02.17 svn.r2891 for OlexSys, GUI svn.r4773)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   40.7892(6)
_cell_length_b                   27.4170(4)
_cell_length_c                   15.0785(2)
_cell_measurement_reflns_used    16372
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      75.6199
_cell_measurement_theta_min      2.1645
_cell_volume                     16862.6(4)
_computing_cell_refinement
;
CrysAlisPro, version 1.171.36.20 (Agilent Technologies, 2012)
;
_computing_data_collection
;
CrysAlisPro, version 1.171.36.32 (Agilent Technologies, 2012)
;
_computing_data_reduction
;
CrysAlisPro, version 1.171.36.20 (Agilent Technologies, 2012)
;
_computing_molecular_graphics
;
<i>Mercury</i> (Macrae et al., 2006)
;
_computing_publication_material
; 
Olex2 (Dolomanov et al., 2009), <i>PLATON for Windows</i> (Spek, 2003) and
<i>publCIF</i> (Westrip, 2010)
;
_computing_structure_refinement  ' SHELXL2013 (Sheldrick, 2008)'
_computing_structure_solution    ' SHELXL97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      160(1)
_diffrn_detector_area_resol_mean 10.3801
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0364467000
_diffrn_orient_matrix_UB_12      -0.0019674000
_diffrn_orient_matrix_UB_13      -0.0266578000
_diffrn_orient_matrix_UB_21      -0.0098737000
_diffrn_orient_matrix_UB_22      0.0138921000
_diffrn_orient_matrix_UB_23      0.0953263000
_diffrn_orient_matrix_UB_31      0.0012188000
_diffrn_orient_matrix_UB_32      0.0543930000
_diffrn_orient_matrix_UB_33      -0.0253174000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0188
_diffrn_reflns_av_unetI/netI     0.0166
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -49
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25977
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.252
_diffrn_reflns_theta_min         3.516
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.795
_exptl_absorpt_correction_T_max  0.814
_exptl_absorpt_correction_T_min  0.553
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_description       plate
_exptl_crystal_F_000             7952
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
(replace by semicolon in column 1 when used as .sqf)
TITL sg1401    F d d 2      R = 0.07
CELL   40.7892   27.4170   15.0786     90.00     90.00     90.00
SPGR Fdd2
C101 0.750 0.250 0.438 !       3.12 eA-3
C102 0.750 0.248 0.297 !       2.63 eA-3
C103 0.331 0.337 0.204 !       1.68 eA-3
C104 0.226 0.247 0.089 !       1.63 eA-3
C105 0.349 0.337 0.155 !       1.56 eA-3
C106 0.184 0.194 0.173 !       1.54 eA-3
C107 0.380 0.073 0.324 !       1.49 eA-3
C108 0.185 0.213 0.097 !       1.49 eA-3
C109 0.792 0.252 0.491 !       1.48 eA-3
C110 0.099 0.150 0.182 !       1.43 eA-3
C111 0.150 0.362 0.471 !       1.13 eA-3
C112 0.100 0.485 0.437 !       0.82 eA-3
Q113 0.253 0.045 0.340 !       0.79 eA-3
Q114 0.850 0.235 0.206 !       0.79 eA-3
C115 0.138 0.193 0.205 !       0.78 eA-3
Q116 0.261 0.423 0.409 !       0.74 eA-3
C117 0.403 0.314 0.173 !       0.67 eA-3
C118 0.429 0.306 0.251 !       0.65 eA-3
Q119 0.234 0.252 0.416 !       0.57 eA-3
Q120 0.748 0.048 0.060 !       0.54 eA-3
Q121 0.249 0.280 0.454 !       0.53 eA-3
Q122 0.271 0.066 0.400 !       0.52 eA-3
(replace by semicolon in column 1 when used as .sqf)
;
_refine_diff_density_max         0.809
_refine_diff_density_min         -0.704
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details
;
 Flack x determined using 3343 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.019(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         7617
_refine_ls_number_restraints     556
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0549P)^2^+62.2984P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1003
_refine_ls_wR_factor_ref         0.1028
_reflns_Friedel_coverage         0.896
_reflns_Friedel_fraction_full    0.973
_reflns_Friedel_fraction_max     0.971
_reflns_number_gt                7295
_reflns_number_total             7617
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic501946f_si_002.cif
_cod_data_source_block           4b_CCDC_993297
_cod_database_code               4341408
_shelxl_version_number           2013-4
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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
2. Restrained distances
 C27-C28A = C27-C28B
 1.5 with sigma of 0.01
 C29A-C34A \\sim C29B-C34B \\sim C33A-C35A \\sim C33B-C35B
 with sigma of 0.005
 C31A-Br2A \\sim C31B-Br2B
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
C28A \\sim C29A \\sim C30A \\sim C31A \\sim C32A \\sim C33A \\sim C28B \\sim
C29B \\sim C30B \\sim C31B \\sim C32B \\sim C33B \\sim C34A \\sim C34B \\sim
C35A \\sim C35B: within 3A with sigma of 0.005 and sigma for terminal atoms of
0.01
Uanis(Br2A) = Uanis(Br2B)
4. Others
 Sof(Br2B)=Sof(C28B)=Sof(C29B)=Sof(C30B)=Sof(H30B)=Sof(C31B)=Sof(C32B)=
 Sof(H32B)=Sof(C33B)=Sof(C34B)=Sof(H34A)=Sof(H34B)=Sof(H34C)=Sof(C35B)=
 Sof(H35D)=Sof(H35E)=Sof(H35F)=1-FVAR(1)
 Sof(Br2A)=Sof(C28A)=Sof(C29A)=Sof(C30A)=Sof(H30A)=Sof(C31A)=Sof(C32A)=
 Sof(H32A)=Sof(C33A)=Sof(C34A)=Sof(H34D)=Sof(H34E)=Sof(H34F)=Sof(C35A)=
 Sof(H35A)=Sof(H35B)=Sof(H35C)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C6(H6), C10(H10), C13(H13), C14(H14), C17(H17), C18(H18), C19(H19),
 C22(H22), C25(H25), C26(H26), C30A(H30A), C32A(H32A), C30B(H30B), C32B(H32B)
5.b Fitted hexagon refined as free rotating group:
 C28A(C29A,C30A,C31A,C32A,C33A), C28B(C29B,C30B,C31B,C32B,C33B)
5.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C34A(H34D,H34E,H34F), C34B(H34A,H34B,H34C),
 C35A(H35A,H35B,H35C), C35B(H35D,H35E,H35F)
;
_shelx_res_checksum              42260
_shelx_hkl_checksum              33847
_shelx_fab_checksum              63661
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS-1997 (Sheldrick, 2008)'