Towards the molecular Borromean link with three unequal rings: double-threaded ruthenium(ii) ring-in-ring complexes
Veliks, Janis; Seifert, Helen M.; Frantz, Derik K.; Klosterman, Jeremy K.; Tseng, Jui-Chang; Linden, Anthony; Siegel, Jay S.; Organic Chemistry Frontiers 3 (2016) 667–; doi:10.1039/C6QO00025H

data_1553427
_publ_section_title
;
 Towards the molecular Borromean link with three unequal rings:
 double-threaded ruthenium(ii) ring-in-ring complexes
;
_journal_issue                   6
_journal_name_full               'Organic Chemistry Frontiers'
_journal_page_first              667
_journal_paper_doi               10.1039/C6QO00025H
_journal_volume                  3
_journal_year                    2016
_chemical_formula_moiety
'C152 H144 N12 O16 Ru2 4+, 4(F6 P 1-), 2(C4 H10 O), 10(C2 H3 N)'
_chemical_formula_sum            'C180 H194 F24 N22 O18 P4 Ru2'
_chemical_formula_weight         3735.50
_chemical_temperature_decomposition_gt 568
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             13-Mar-2012
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-10-15 deposited with the CCDC.
2016-02-22 downloaded from the CCDC.
;
_cell_angle_alpha                71.0730(10)
_cell_angle_beta                 82.6220(10)
_cell_angle_gamma                68.2880(10)
_cell_formula_units_Z            1
_cell_length_a                   13.6711(2)
_cell_length_b                   16.9670(2)
_cell_length_c                   22.4266(3)
_cell_measurement_reflns_used    30412
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      72.4735
_cell_measurement_theta_min      2.0810
_cell_volume                     4571.45(11)
_computing_cell_refinement
'CrysAlisPro, Version 1.171.35.19 (Agilent Technologies, 2011)'
_computing_data_collection
'CrysAlisPro, Version 1.171.35.19 (Agilent Technologies, 2011)'
_computing_data_reduction
'CrysAlisPro, Version 1.171.35.19 (Agilent Technologies, 2011)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  'SHELXL97 and PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      160(1)
_diffrn_detector                 'Atlas CCD camera on \k goniostat'
_diffrn_detector_area_resol_mean 10.3801
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type
'Oxford Diffraction SuperNova, dual radiation diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_sigmaI/netI    0.0296
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            54280
_diffrn_reflns_theta_full        66.97
_diffrn_reflns_theta_max         72.62
_diffrn_reflns_theta_min         2.08
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.453
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69216
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
CrysAlisPro, Version 1.171.35.19 (Agilent Technologies, 2011)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1936
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;
Note that this work was conducted in 2012, before the appearance of 
SHELXL-2013 and thus the 'old style' of SQUEEZE is used here.
;
_refine_diff_density_max         2.360
_refine_diff_density_min         -0.872
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1145
_refine_ls_number_reflns         17661
_refine_ls_number_restraints     505
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0803
_refine_ls_R_factor_gt           0.0690
_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^)+(0.1388P)^2^+3.5799P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2021
_refine_ls_wR_factor_ref         0.2134
_reflns_number_gt                14735
_reflns_number_total             17661
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6qo00025h2.cif
_cod_data_source_block           13
_cod_depositor_comments
;
The following automatic conversions were performed:

data name '_chemical_melting_point' was changed to
'_chemical_temperature_decomposition_gt' since the value was
specified as 'more than' ('>') a certain temperature. The value ' >
568 K, dec.' was changed to '568' -- it should be numeric and without
a unit designator.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               1553427