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_4349169
_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
'C34 H22 Br2 N6 Ru, 2(F6 P), 0.5(C2 H6 O), 0.5(H2 O)'
_chemical_formula_sum            'C35 H26 Br2 F12 N6 O P2 Ru'
_chemical_formula_weight         1097.44
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-01-26
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-01-26 # Formatted by publCIF

;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.237(4)
_cell_length_b                   32.482(7)
_cell_length_c                   12.878(3)
_cell_measurement_reflns_used    12179
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.1
_cell_measurement_theta_min      1.25
_cell_volume                     7629(3)
_computing_cell_refinement       'BluIce (McPhillips, 2002)'
_computing_data_collection       'XDS (Kabsch, 1993)'
_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
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  'ADSC Quantum 315r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0522
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            157148
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.100
_diffrn_reflns_theta_min         1.254
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.690
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.911
_exptl_crystal_description       block
_exptl_crystal_F_000             4304
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.012
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.768
_refine_diff_density_min         -1.735
_refine_diff_density_rms         0.128
_refine_ls_abs_structure_details
;
 Flack x determined using 9050 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.0279(18)
_refine_ls_extinction_coef       0.00050(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1069
_refine_ls_number_reflns         21456
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0480
_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^)+(0.0705P)^2^+18.8311P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1249
_refine_ls_wR_factor_ref         0.1262
_reflns_Friedel_coverage         0.849
_reflns_Friedel_fraction_full    0.974
_reflns_Friedel_fraction_max     0.959
_reflns_number_gt                20676
_reflns_number_total             21456
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            delta-[Ru(phen)2(2)](PF6)2.cif
_cod_data_source_block           p21_a
_cod_depositor_comments
;

2020-05-08
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '2(C34 H22 Br2 N6 Ru), 4(F6 P), C2 H6 O, H2 O'
_cod_original_formula_sum        'C70 H52 Br4 F24 N12 O2 P4 Ru2'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     2194.89
_cod_database_code               4349169
_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) groups, All O(H,H) groups
2. Rigid body (RIGU) restrains
 P4, F20, F21, F22, F23, F24, F25
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Free rotating group:
 O2(H2A,H2B)
3.b Secondary CH2 refined with riding coordinates:
 C36(H36A,H36B)
3.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C13(H13),
 C14(H14), C15(H15), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C25(H25),
  C27(H27), C28(H28), C31(H31), C32(H32), C34(H34), C1'(H1'), C2'(H2'),
 C3'(H3'), C5'(H5'), C6'(H6'), C8'(H8'), C9'(H9'), C10'(H10'), C13'(H13'),
 C14'(H14'), C15'(H15'), C17'(H17'), C18'(H18'), C20'(H20'), C21'(H21'),
 C22'(H22'), C25'(H25'), C27'(H27'), C28'(H28'), C31'(H31'), C32'(H32'),
 C34'(H34')
3.d Idealised Me refined as rotating group:
 C35(H35B,H35A,H35C)
3.e Idealised tetrahedral OH refined as rotating group:
 O1(H1A)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'