From Nano-Balls to Nano-Bowls
Brake, Helena; Presypkina, Eugenia V.; Heindl, Claudia; Virovets, Alexander Viktorovich; Kremer, Werner; Scheer, Manfred; Chemical Science  (2019) –; doi:10.1039/C8SC05471A

data_1550516
_publ_section_title
;
 From Nano-Balls to Nano-Bowls
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C8SC05471A
_journal_year                    2019
_chemical_formula_moiety
'C110 H165 Br14.55 Cu14.55 Fe11 P55, C10 H10 As5 Cr2, 3.4(C H2 Cl2),  0.9 (C H3 C N)'
_chemical_formula_structural
'((Cp Cr)2 As5)@[(Cp* Fe P5)11 (Cu Br)14.55] * 3.4 (C H2 Cl2) * 0.9 (Me C N)'
_chemical_formula_sum
'C125.2 H184.5 As5 Br14.55 Cl6.8 Cr2 Cu14.55 Fe11 N0.9 P55'
_chemical_formula_weight         6826.78
_chemical_melting_point          layering
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-10-24 deposited with the CCDC.
2019-01-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.3511(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.08802(13)
_cell_length_b                   33.62013(12)
_cell_length_c                   25.36593(11)
_cell_measurement_reflns_used    116918
_cell_measurement_temperature    80(2)
_cell_measurement_theta_max      31.4670
_cell_measurement_theta_min      1.7060
_cell_volume                     22476.48(17)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1998)'
_diffrn_ambient_temperature      80(2)
_diffrn_detector                 'pixel array detectot'
_diffrn_detector_type            'Dectris PILATUS 6M'
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.754
_diffrn_measurement_device       'one-circle diffractometer'
_diffrn_measurement_device_type
'P11 beamline, PETRA III, DESY, Dectris PILATUS 6M'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6199
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_unetI/netI     0.0453
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.754
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            256480
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.754
_diffrn_reflns_theta_full        21.925
_diffrn_reflns_theta_max         31.571
_diffrn_reflns_theta_min         1.713
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    4.113
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86794
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.017
_exptl_crystal_description       rod
_exptl_crystal_F_000             13251
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.050
_refine_diff_density_max         2.029
_refine_diff_density_min         -1.262
_refine_diff_density_rms         0.164
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.043(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2251
_refine_ls_number_reflns         81064
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0395
_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^)+(0.0689P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1057
_refine_ls_wR_factor_ref         0.1076
_reflns_Friedel_coverage         0.999
_reflns_Friedel_fraction_full    0.965
_reflns_Friedel_fraction_max     0.754
_reflns_number_gt                64901
_reflns_number_total             81064
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc05471a2.cif
_cod_data_source_block           novac
_cod_original_cell_volume        22476.47(17)
_cod_original_formula_sum
'C125.20 H184.50 As5 Br14.55 Cl6.80 Cr2 Cu14.55 Fe11 N0.90 P55'
_cod_database_code               1550516
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.577
_shelx_estimated_absorpt_t_max   0.821
_oxdiff_exptl_absorpt_empirical_full_min 0.902
_oxdiff_exptl_absorpt_empirical_full_max 1.111
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              19451