Conformations of large macrocycles and ring-in-ring complexes
Klosterman, Jeremy K.; Veliks, Janis; Frantz, Derik K.; Yasui, Yoshizumi; Loepfe, Michael; Zysman-Colman, Eli; Linden, Anthony; Siegel, Jay S.; Organic Chemistry Frontiers 3 (2016) 661–; doi:10.1039/C6QO00024J

data_1553422
_publ_section_title
;
 Conformations of large macrocycles and ring-in-ring complexes
;
_journal_issue                   6
_journal_name_full               'Organic Chemistry Frontiers'
_journal_page_first              661
_journal_paper_doi               10.1039/C6QO00024J
_journal_volume                  3
_journal_year                    2016
_chemical_formula_moiety
'C178 H166 N18 O12 Ru2 4+, 4(F6 P -), 12(C6 H6)'
_chemical_formula_sum            'C250 H238 F24 N18 O12 P4 Ru2'
_chemical_formula_weight         4468.59
_space_group_crystal_system      orthorhombic
_space_group_IT_number           48
_space_group_name_Hall           '-P 2ab 2bc'
_space_group_name_H-M_alt        'P n n n :2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-11-17 deposited with the CCDC.
2016-03-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.8240(10)
_cell_length_b                   22.5830(10)
_cell_length_c                   47.8130(10)
_cell_measurement_temperature    100(1)
_cell_volume                     24644.5(16)
_computing_cell_refinement       'Swiss Light Source PX beam line software'
_computing_data_collection       'Swiss Light Source PX beam line software'
_computing_data_reduction        'Swiss Light Source PX beam line software'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  'SHELXL-2014/7 and PLATON (Spek, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 0.678
_diffrn_measured_fraction_theta_max 0.678
_diffrn_measurement_device_type  'MarResearch 225 detector'
_diffrn_measurement_method       'phi scan'
_diffrn_radiation_type           'synchrotron X-rays'
_diffrn_radiation_wavelength     0.8000
_diffrn_reflns_av_R_equivalents  0.048
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_Laue_measured_fraction_full 0.678
_diffrn_reflns_Laue_measured_fraction_max 0.678
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            93055
_diffrn_reflns_point_group_measured_fraction_full 0.678
_diffrn_reflns_point_group_measured_fraction_max 0.678
_diffrn_reflns_theta_full        27.501
_diffrn_reflns_theta_max         27.501
_diffrn_reflns_theta_min         2.315
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.309
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             9296
_platon_squeeze_details
;
Further details included in the .fab section right at the end of this CIF.
;
_refine_diff_density_max         1.190
_refine_diff_density_min         -0.647
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.178
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1087
_refine_ls_number_reflns         13465
_refine_ls_number_restraints     852
_refine_ls_restrained_S_all      2.243
_refine_ls_R_factor_all          0.1750
_refine_ls_R_factor_gt           0.1536
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4615
_refine_ls_wR_factor_ref         0.4940
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9226
_reflns_number_total             13465
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6qo00024j2.cif
_cod_data_source_block           2-terpy
_cod_original_sg_symbol_H-M      'P n n n'
_cod_database_code               1553422
_shelx_shelxl_version_number     2014/7
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              41564
_shelx_fab_checksum              86130