CCCCC pentadentate chelates with planar Mobius aromaticity and unique properties
Congqing Zhu; Caixia Yang; Yongheng Wang; Gan Lin; Yuhui Yang; Xiaoyong Wang; Jun Zhu; Xiaoyuan Chen; Xin Lu; Gang Liu; Haiping Xia; Science Advances 2 (2016) 1601031–; doi:10.1126/sciadv.1601031

data_1548343
_publ_section_title
;
 CCCCC pentadentate chelates with planar Mobius aromaticity and unique
 properties
;
_journal_name_full               'Science Advances'
_journal_page_first              1601031
_journal_paper_doi               10.1126/sciadv.1601031
_journal_volume                  2
_journal_year                    2016
_chemical_formula_moiety         'C68 H58 Os P3, B F4, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C68.5 H59 B Cl F4 Os P3'
_chemical_formula_weight         1287.52
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_cell_angle_alpha                108.68(3)
_cell_angle_beta                 96.47(3)
_cell_angle_gamma                96.12(3)
_cell_formula_units_Z            4
_cell_length_a                   9.938(2)
_cell_length_b                   24.307(5)
_cell_length_c                   25.357(5)
_cell_measurement_reflns_used    10019
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      54.98
_cell_measurement_theta_min      6.04
_cell_volume                     5699(2)
_computing_cell_refinement       RAPID-AUTO
_computing_data_collection       'RAPID-AUTO (Rigaku Corporation, 1998)'
_computing_data_reduction
'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2002)'
_computing_molecular_graphics    'XP (Sheldrick, 1993)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0954
_diffrn_reflns_av_sigmaI/netI    0.0952
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            61305
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.00
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.425
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4115
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2596
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.556
_refine_diff_density_min         -2.261
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1414
_refine_ls_number_reflns         19461
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0796
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0478P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0993
_refine_ls_wR_factor_ref         0.1086
_reflns_number_gt                13930
_reflns_number_total             19461
_reflns_threshold_expression     >2sigma(I)
_cod_depositor_comments
;

2019-01-13
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C137 H118 B2 Cl2 F8 Os2 P6'
_cod_original_formula_weight         2575.05
_cod_original_formula_moiety         '2(C68 H58 Os P3),2(BF4),CH2Cl2'
_cod_original_formula_units_Z            2
_cod_data_source_file            2e.cif
_cod_data_source_block           1
_cod_database_code               1548343