Crystallographic Characterization of Lu2C2n (2n = 76-90): Cluster Selection by Cage Size
Lu, Xing; Shen, Wangqiang; Bao, Lipiao; Hu, Shuaifeng; Yang, Le; Jin, Peng; Xie, Yun-Peng; Akasaka, Takeshi; Chemical Science  (2019) –; doi:10.1039/C8SC03886D

data_1550158
_publ_section_title
;
 Crystallographic Characterization of Lu2C2n (2n = 76-90): Cluster
 Selection by Cage Size
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C8SC03886D
_journal_year                    2019
_chemical_formula_moiety
'Lu2 C90, C36 H44 N4 Ni, 1.6(C6 H6), 0.4(C S2)'
_chemical_formula_sum            'C136 H53.6 Lu2 N4 Ni S0.8'
_chemical_formula_weight         2177.69
_chemical_name_common            'Lu2C2@Cs-C88 Ni(OEP)'
_chemical_name_systematic        'Lu2C2@Cs-C88 Ni(OEP)'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-04-13 deposited with the CCDC.
2018-10-29 downloaded from the CCDC.
;
_cell_angle_alpha                84.624(5)
_cell_angle_beta                 88.620(5)
_cell_angle_gamma                62.644(5)
_cell_formula_units_Z            2
_cell_length_a                   14.749(5)
_cell_length_b                   15.029(5)
_cell_length_c                   19.899(5)
_cell_measurement_reflns_used    9723
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.127
_cell_measurement_theta_min      2.503
_cell_volume                     3899(2)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.914
_diffrn_measured_fraction_theta_max 0.913
_diffrn_measurement_device_type  'CCD MX300-HE'
_diffrn_measurement_method       'phi scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6525
_diffrn_reflns_av_R_equivalents  0.0703
_diffrn_reflns_av_unetI/netI     0.0691
_diffrn_reflns_Laue_measured_fraction_full 0.914
_diffrn_reflns_Laue_measured_fraction_max 0.913
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            44643
_diffrn_reflns_point_group_measured_fraction_full 0.914
_diffrn_reflns_point_group_measured_fraction_max 0.913
_diffrn_reflns_theta_full        23.048
_diffrn_reflns_theta_max         23.154
_diffrn_reflns_theta_min         0.944
_diffrn_source                   'SSRF, Beamline BL17B'
_exptl_absorpt_coefficient_mu    2.309
_exptl_absorpt_correction_T_max  0.7449
_exptl_absorpt_correction_T_min  0.4105
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.855
_exptl_crystal_description       Block
_exptl_crystal_F_000             2161
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.917
_refine_diff_density_min         -2.525
_refine_diff_density_rms         0.210
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1466
_refine_ls_number_reflns         13054
_refine_ls_number_restraints     1714
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0991
_refine_ls_R_factor_gt           0.0916
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1659P)^2^+37.0596P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2540
_refine_ls_wR_factor_ref         0.2637
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11440
_reflns_number_total             13054
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc03886d2.cif
_cod_data_source_block           Lu2C2@Cs-C88
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_formula_sum        'C136 H53.60 Lu2 N4 Ni S0.80'
_cod_database_code               1550158
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.758
_shelx_estimated_absorpt_t_max   0.831
_shelx_res_checksum              63065