A lens-shaped supramolecule based on the bulky pentaphosphaferrocene [CpBIGFe(η5-P5)] and CuBr2
Heinl, Sebastian; Peresypkina, Eugenia V.; Kremer, Werner; Scheer, Manfred; Chemical Communications  (2023) –; doi:10.1039/D3CC03244B

data_7131925
_publ_section_title
;
 A lens-shaped supramolecule based on the bulky pentaphosphaferrocene
 [CpBIGFe(\h5-P5)] and CuBr2
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC03244B
_journal_year                    2023
_chemical_formula_moiety         'C342 H408 Br32 Cu32 Fe6 N6 P30, 2.4(C H2 Cl2)'
_chemical_formula_structural
'[(C55 H65 Fe P5)6 {Cu Br}32 (C H3 C N)6] * 2.4(C H2 Cl2)'
_chemical_formula_sum            'C344.4 H412.8 Br32 Cl4.8 Cu32 Fe6 N6 P30'
_chemical_formula_weight         10661.14
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-03-02 deposited with the CCDC.	2023-07-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   30.0348(4)
_cell_length_b                   30.0348(4)
_cell_length_c                   38.1116(9)
_cell_measurement_reflns_used    30191
_cell_measurement_temperature    123.02(10)
_cell_measurement_theta_max      72.2990
_cell_measurement_theta_min      3.5690
_cell_volume                     29774.0(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SIR-97 (Altomare, 1999)'
_diffrn_ambient_temperature      123.02(10)
_diffrn_detector_area_resol_mean 10.3546
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            71417
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.488
_diffrn_reflns_theta_max         67.488
_diffrn_reflns_theta_min         3.479
_exptl_absorpt_coefficient_mu    9.061
_exptl_absorpt_correction_T_max  0.648
_exptl_absorpt_correction_T_min  0.521
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.784
_exptl_crystal_description       prism
_exptl_crystal_F_000             15770
_exptl_crystal_size_max          0.1088
_exptl_crystal_size_mid          0.0682
_exptl_crystal_size_min          0.0680
_refine_diff_density_max         1.354
_refine_diff_density_min         -0.855
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     900
_refine_ls_number_reflns         11894
_refine_ls_number_restraints     124
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0492
_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^)+(0.0816P)^2^+486.2281P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1553
_refine_ls_wR_factor_ref         0.1581
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10124
_reflns_number_total             11894
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc03244b2.cif
_cod_data_source_block           last
_cod_original_cell_volume        29774.0(11)
_cod_original_formula_sum        'C344.40 H412.80 Br32 Cl4.80 Cu32 Fe6 N6 P30'
_cod_database_code               7131925
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              27164
_shelx_hkl_checksum              45635