Generation of a zinc and rhodium containing metallomacrocycle by rearrangement of a six-coordinate precursor complex.
Groß, C; Sun, Y.; Jost, T.; Grimm, T.; Klein, M. P.; Niedner-Schatteburg, G; Becker, S.; Thiel, W. R.; Chemical communications (Cambridge, England) 56 (2020) 368–371; doi:10.1039/c9cc07723e

data_7125455
_publ_section_title
;
 Generation of a zinc and rhodium containing metallomacrocycle by
 rearrangement of a six-coordinate precursor complex.
;
_journal_issue                   3
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              368
_journal_page_last               371
_journal_paper_doi               10.1039/c9cc07723e
_journal_volume                  56
_journal_year                    2020
_chemical_formula_sum            'C123 H124 B Cl6 F7 N10 O6 P4 Rh2 S Zn'
_chemical_formula_weight         2621.95
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2019-09-17 deposited with the CCDC.	2019-11-26 downloaded from the CCDC.
;
_cell_angle_alpha                90.780(2)
_cell_angle_beta                 106.494(2)
_cell_angle_gamma                109.253(2)
_cell_formula_units_Z            2
_cell_length_a                   15.3537(3)
_cell_length_b                   19.4633(4)
_cell_length_c                   22.6951(5)
_cell_measurement_reflns_used    24501
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      62.6570
_cell_measurement_theta_min      4.0730
_cell_volume                     6096.0(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SIR92 (Giacovazzo et al., 1994)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 16.1399
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_av_unetI/netI     0.0400
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            51266
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        62.743
_diffrn_reflns_theta_max         62.743
_diffrn_reflns_theta_min         3.202
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    4.824
_exptl_absorpt_correction_T_max  0.669
_exptl_absorpt_correction_T_min  0.423
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_description       'transparent prism'
_exptl_crystal_F_000             2692
_exptl_crystal_size_max          0.358
_exptl_crystal_size_mid          0.238
_exptl_crystal_size_min          0.123
_refine_diff_density_max         4.146
_refine_diff_density_min         -1.314
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1702
_refine_ls_number_reflns         19392
_refine_ls_number_restraints     3547
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0525
_refine_ls_shift/su_max          8.891
_refine_ls_shift/su_mean         0.064
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0976P)^2^+12.3029P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1525
_refine_ls_wR_factor_ref         0.1599
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16392
_reflns_number_total             19392
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc07723e2.cif
_cod_data_source_block           shelx_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7125454--7125455.cif.'
_cod_database_code               7125455
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.277
_shelx_estimated_absorpt_t_max   0.588
_shelx_res_checksum              64838