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_1550515
_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 Cl13.35 Cu13.35 Fe11 P55, C10 H10 As5 Cr2, 2.96(C H2 Cl2),  3.825 (C H3 C N)'
_chemical_formula_structural
'((Cp Cr)2 As5)@[(Cp* Fe P5)11 (Cu Cl)13.35] * 2.96(C H2 Cl2) * 3.825(Me C N)'
_chemical_formula_sum
'C130.61 H192.4 As5 Cl19.27 Cr2 Cu13.35 Fe11 N3.83 P55'
_chemical_formula_weight         6143.82
_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                 112.8750(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   30.4118(4)
_cell_length_b                   29.4289(2)
_cell_length_c                   28.8188(3)
_cell_measurement_reflns_used    37353
_cell_measurement_temperature    123.0(3)
_cell_measurement_theta_max      74.2290
_cell_measurement_theta_min      3.1230
_cell_volume                     23764.0(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.37b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.37b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.37b (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1998)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.0(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.1818
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1091
_diffrn_reflns_av_unetI/netI     0.0780
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            83809
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         74.244
_diffrn_reflns_theta_min         3.003
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.739
_exptl_absorpt_correction_T_max  0.651
_exptl_absorpt_correction_T_min  0.239
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.37b (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.717
_exptl_crystal_description       rod
_exptl_crystal_F_000             12166
_exptl_crystal_size_max          0.185
_exptl_crystal_size_mid          0.063
_exptl_crystal_size_min          0.038
_refine_diff_density_max         1.509
_refine_diff_density_min         -1.311
_refine_diff_density_rms         0.175
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.043(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2341
_refine_ls_number_reflns         31627
_refine_ls_number_restraints     117
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0562
_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^)+(0.0927P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1412
_refine_ls_wR_factor_ref         0.1445
_reflns_Friedel_coverage         0.999
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.968
_reflns_number_gt                26711
_reflns_number_total             31629
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc05471a2.cif
_cod_data_source_block           new
_cod_original_formula_sum
'C130.61 H192.40 As5 Cl19.27 Cr2 Cu13.35 Fe11 N3.83 P55'
_cod_database_code               1550515
_shelx_shelxl_version_number     2014/7
_oxdiff_exptl_absorpt_empirical_full_min 0.340
_oxdiff_exptl_absorpt_empirical_full_max 2.909
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              7201