Chiral Ruthenium(II) Complexes as Supramolecular Building Blocks for Heterometallic Self-Assembly.
Iranmanesh, Hasti; Arachchige, Kasun S. A.; Bhadbhade, Mohan; Donald, William A.; Liew, Jane Y.; Liu, Kenny T.-C.; Luis, Ena T.; Moore, Evan G.; Price, Jason R.; Yan, Hong; Yang, Jiajia; Beves, Jonathon E.; Inorganic chemistry 55 (2016) 12737–12751; doi:10.1021/acs.inorgchem.6b02007

data_4349172
_publ_section_title
;
 Chiral Ruthenium(II) Complexes as Supramolecular Building Blocks for
 Heterometallic Self-Assembly.
;
_journal_issue                   24
_journal_name_full               'Inorganic chemistry'
_journal_page_first              12737
_journal_page_last               12751
_journal_paper_doi               10.1021/acs.inorgchem.6b02007
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety
'4(C44 H30 N8 Ru), 8(F6 P), C4 H10 O, 2(H2 O)'
_chemical_formula_sum            'C180 H134 F48 N32 O3 P8 Ru4'
_chemical_formula_weight         4357.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-03-07
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.16 svn.r3265 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-03-07 # Formatted by publCIF
;
_cell_angle_alpha                90
_cell_angle_beta                 95.94(3)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   12.638(3)
_cell_length_b                   23.853(5)
_cell_length_c                   16.772(3)
_cell_measurement_reflns_used    1290
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.94
_cell_measurement_theta_min      1.22
_cell_volume                     5028.8(18)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_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(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0630
_diffrn_reflns_av_unetI/netI     0.0497
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            84624
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.939
_diffrn_reflns_theta_min         1.221
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_exptl_absorpt_coefficient_mu    0.461
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_description       plate
_exptl_crystal_F_000             2190
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.035
_exptl_crystal_size_min          0.024
_refine_diff_density_max         0.513
_refine_diff_density_min         -1.134
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details
;
 Flack x determined using 8012 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.001(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1296
_refine_ls_number_reflns         23185
_refine_ls_number_restraints     289
_refine_ls_restrained_S_all      1.175
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0494
_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^)+(0.0869P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1232
_refine_ls_wR_factor_ref         0.1302
_reflns_Friedel_coverage         0.939
_reflns_Friedel_fraction_full    0.964
_reflns_Friedel_fraction_max     0.953
_reflns_number_gt                19264
_reflns_number_total             23185
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            delta-[Ru(phen)2(4)](PF6)2.cif
_cod_data_source_block           p21_a
_cod_database_code               4349172
_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,H) groups
2. Restrained distances
 O2-H2A = O2-H2B
 0.9584 with sigma of 0.001
 H2A-H2B
 1.515 with sigma of 0.001
 C16-C17 \\sim C18-N8 \\sim C19-C20
 with sigma of 0.02
3. Restrained planarity
 N8, C16, C17, C18, C19, C20
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(F9) = Uanis(F8)
Uanis(F10) = Uanis(F14)
Uanis(F12) = Uanis(F13)
Uanis(F16) = Uanis(F11)
Uanis(F3) = Uanis(F3A)
Uanis(F3AA) = Uanis(F3AB)
Uanis(F5) = Uanis(F5A)
Uanis(F2) = Uanis(F2A)
Uanis(F2AA) = Uanis(F2AB)
Uanis(F1) = Uanis(F1A)
5. Rigid body (RIGU) restrains
 P2, F7, F8, F9, F10, F11, F12, F13, F14, F15, F16
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N8, C16, C17, C18, C19, C20
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 P0AA, F1, F1A, F2, F2A, F2AA, F2AB, F3, F3A, F3AA, F3AB, F5, F5A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: F1(0.55364) F1A(0.44636) F2(0.55666) F2A(0.44334) F2AA(0.5981)
 F2AB(0.4019) F3(0.53398) F3A(0.46602) F3AA(0.50679) F3AB(0.49321) F5(0.58409)
 F5A(0.41591) F8(0.46538) F9(0.53462) F10(0.50225) F11(0.43712) F12(0.55504)
 F13(0.44496) F14(0.49775) F16(0.56288) O1(0.5) C89(0.5) H89A(0.5) H89B(0.5)
 H89C(0.5) C90(0.5) H90A(0.5) H90B(0.5) C91(0.5) H91A(0.5) H91B(0.5) C92(0.5)
 H92A(0.5) H92B(0.5) H92C(0.5)
7.a Free rotating group:
 O2(H2A,H2B)
7.b Secondary CH2 refined with riding coordinates:
 C90(H90A,H90B), C91(H91A,H91B)
7.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C3AA(H3AA), C4(H4), C4AA(H4AA), C8(H8), C9(H9), C12(H12),
 C13(H13), C14(H14), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22),
  C23(H23), C26(H26), C27(H27), C30(H30), C31(H31), C32(H32), C33(H33),
 C34(H34), C35(H35), C40(H40), C41(H41), C42(H42), C43(H43), C44(H44), C45(H45),
  C46(H46), C47(H47), C48(H48), C51(H51), C52(H52), C53(H53), C56(H56),
 C57(H57), C59(H59), C61(H61), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66),
  C67(H67), C72(H72), C73(H73), C74(H74), C75(H75), C76(H76), C77(H77),
 C78(H78), C79(H79), C84(H84), C85(H85), C86(H86), C87(H87), C88(H88)
7.d Idealised Me refined as rotating group:
 C89(H89A,H89B,H89C), C92(H92A,H92B,H92C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'