Chiral macrocyclic terpyridine complexes.
Brandl, Thomas; Hoffmann, Viktor; Pannwitz, Andrea; Häussinger, Daniel; Neuburger, Markus; Fuhr, Olaf; Bernhard, Stefan; Wenger, Oliver S.; Mayor, Marcel; Chemical science 9 (2018) 3837–3843; doi:10.1039/c7sc05285e

data_1549124
_publ_section_title
;
 Chiral macrocyclic terpyridine complexes.
;
_journal_issue                   15
_journal_name_full               'Chemical science'
_journal_page_first              3837
_journal_page_last               3843
_journal_paper_doi               10.1039/c7sc05285e
_journal_volume                  9
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C62 H34 N6 Ru, 2(F6 P), C4 H10 O'
_chemical_formula_sum            'C66 H44 F12 N6 O P2 Ru'
_chemical_formula_weight         1328.08
_space_group_crystal_system      tetragonal
_space_group_IT_number           114
_space_group_name_Hall           'P -4 2n'
_space_group_name_H-M_alt        'P -4 21 c'
_symmetry_space_group_name_Hall  'P -4 2n'
_symmetry_space_group_name_H-M   'P -4 21 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-11-17
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_audit_update_record
;
2017-02-21 deposited with the CCDC.
2018-03-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.39200(10)
_cell_length_b                   16.39200(10)
_cell_length_c                   21.9038(2)
_cell_measurement_reflns_used    231475
_cell_measurement_temperature    123.0
_cell_measurement_theta_max      57.74
_cell_measurement_theta_min      2.93
_cell_volume                     5885.50(7)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      123.0
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       '4-circle goniometer'
_diffrn_measurement_device_type  'Stoe StadiVari'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '1.2 0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34143
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_unetI/netI     0.0061
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            119994
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        53.597
_diffrn_reflns_theta_max         57.438
_diffrn_reflns_theta_min         2.929
_diffrn_source                   'Metaljet D2'
_diffrn_source_current           2.860
_diffrn_source_power             0.200
_diffrn_source_voltage           70
_exptl_absorpt_coefficient_mu    2.263
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_description       block
_exptl_crystal_F_000             2688
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.536
_refine_diff_density_min         -0.794
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
;
 Flack x determined using 2627 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.018(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         6077
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0335
_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^)+(0.0659P)^2^+3.2323P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0967
_refine_ls_wR_factor_ref         0.0974
_reflns_Friedel_coverage         0.816
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                5942
_reflns_number_total             6077
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc05285e2.cif
_cod_data_source_block           brt235_3_123k
_cod_depositor_comments
'Adding full bibliography for 1549123--1549124.cif.'
_cod_original_cell_volume        5885.50(9)
_cod_database_code               1549124
_shelxl_version_number           2013-4
_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
 O1B-C33B
 2.5 with sigma of 0.02
 O1A-C33A
 2.5 with sigma of 0.02
 O1B-C32B = O1A-C32A
 1.43 with sigma of 0.02
 C33B-C32B = C33A-C32A
 1.54 with sigma of 0.02
3. Others
 Fixed Sof: O1A(0.25) C32A(0.5) H32A(0.5) H32B(0.5) C33A(0.5) H33A(0.5)
 H33B(0.5) H33C(0.5) O1B(0.25) C32B(0.5) H32C(0.5) H32D(0.5) C33B(0.5)
 H33D(0.5) H33E(0.5) H33F(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C32A(H32A,H32B), C32B(H32C,H32D)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C7(H7), C8(H8), C9(H9), C12(H12), C14(H14), C15(H15),
 C18(H18), C19(H19), C20(H20), C21(H21), C28(H28), C29(H29), C30(H30), C31(H31)
4.c Idealised Me refined as rotating group:
 C33A(H33A,H33B,H33C), C33B(H33D,H33E,H33F)
;
_shelx_res_checksum              87982
_shelx_hkl_checksum              87747
_olex2_submission_special_instructions 'No special instructions were received'