Helical fluxionality: numerical frustration drives concerted low-barrier screw motions of a tricopper cluster.
Kim, Heechan; Shin, Juhwan; Kim, Seyong; Lee, Dongwhan; Chemical science 14 (2023) 3265–3269; doi:10.1039/d3sc00851g

data_1568557
_publ_section_title
;
 Helical fluxionality: numerical frustration drives concerted low-barrier
 screw motions of a tricopper cluster.
;
_journal_issue                   12
_journal_name_full               'Chemical science'
_journal_page_first              3265
_journal_page_last               3269
_journal_paper_doi               10.1039/d3sc00851g
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C41 H43 Cu1.5 N7 O2, 3(B0.5 F2), C2 H3 N'
_chemical_formula_sum            'C43 H46 B1.5 Cu1.5 F6 N8 O2'
_chemical_formula_weight         932.40
_chemical_properties_physical    Air-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-09-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-06-12 deposited with the CCDC.	2023-02-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.3040(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   29.3549(2)
_cell_length_b                   14.38170(10)
_cell_length_c                   21.2892(2)
_cell_measurement_reflns_used    20435
_cell_measurement_temperature    93
_cell_measurement_theta_max      78.9820
_cell_measurement_theta_min      3.2220
_cell_volume                     8626.30(12)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      93
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -89.00  24.00   0.50    1.80    --    0.00 -38.00  30.00  226
  2  \w     14.00  52.00   0.50    1.80    --   28.00 -50.00-169.61   76
  3  \w    -58.00   1.00   0.50    1.80    --   28.00 -50.00-169.61  118
  4  \w     21.00  52.00   0.50    1.80    --   44.00 -41.00 100.08   62
  5  \w     98.00 124.00   0.50    3.14    --  105.20 -82.00-180.00   52
  6  \w     92.00 118.00   0.50    3.14    --  105.20 -82.00 -60.00   52
  7  \w     49.00  75.00   0.50    3.14    --  105.20 -82.00-180.00   52
  8  \w     80.00 156.00   0.50    3.14    --  105.20  45.00   0.00  152
  9  \w     38.00 135.00   0.50    3.14    --  105.20 -82.00-150.00  194
 10  \w     66.00 126.00   0.50    3.14    --  105.20 -82.00 -90.00  120
 11  \w     34.00  60.00   0.50    3.14    --  105.20 -82.00 -90.00   52
 12  \w     16.00 133.00   0.50    3.14    --  105.20 -61.00  30.00  234
 13  \w     74.00 195.00   0.50    3.14    --  105.20  15.00 -60.00  242
 14  \w     16.00  57.00   0.50    3.14    --  105.20  15.00 -60.00   82
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0215924000
_diffrn_orient_matrix_UB_12      0.0434739000
_diffrn_orient_matrix_UB_13      0.0679805000
_diffrn_orient_matrix_UB_21      0.0058734000
_diffrn_orient_matrix_UB_22      -0.0976280000
_diffrn_orient_matrix_UB_23      0.0310392000
_diffrn_orient_matrix_UB_31      0.0498920000
_diffrn_orient_matrix_UB_32      -0.0073772000
_diffrn_orient_matrix_UB_33      -0.0099032000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0227
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            27227
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.422
_diffrn_reflns_theta_min         3.137
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.590
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.466
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
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            'clear intense brown'
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_description       block
_exptl_crystal_F_000             3848
_exptl_crystal_recrystallization_method 'Vapour deposition'
_exptl_crystal_size_max          0.389
_exptl_crystal_size_mid          0.245
_exptl_crystal_size_min          0.197
_refine_diff_density_max         1.749
_refine_diff_density_min         -0.901
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     579
_refine_ls_number_reflns         9070
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0565
_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^)+(0.0912P)^2^+23.9295P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1584
_refine_ls_wR_factor_ref         0.1597
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8574
_reflns_number_total             9070
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc00851g1.cif
_cod_data_source_block           jhs-cubf4-oipr
_cod_depositor_comments          'Adding full bibliography for 1568557.cif.'
_cod_original_formula_sum        'C43 H46 B1.50 Cu1.50 F6 N8 O2'
_cod_database_code               1568557
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C43 H46 B1.5 Cu1.5 F6 N8 O2'
_chemical_oxdiff_usercomment     JHS-CuBF4-OiPr
_reflns_odcompleteness_completeness 99.59
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: F01I(0.5) F0AA(0.5)
3.a Ternary CH refined with riding coordinates:
 C01B(H01H), C01D(H01I)
3.b Aromatic/amide H refined with riding coordinates:
 N009(H009), N00E(H00E), C00N(H00N), C00O(H00O), C00R(H00R), C00T(H00T),
 C00U(H00U), C00Y(H00Y), C010(H010), C011(H011), C014(H014), C016(H016),
 C018(H018), C01A(H01G)
3.c Idealised Me refined as rotating group:
 C017(H01A,H01B,H01C), C019(H01D,H01E,H01F), C01E(H01J,H01K,H01L), C01F(H01M,
 H01N,H01O), C01G(H01P,H01Q,H01R), C01H(H01S,H01T,H01U), C01K(H01V,H01W,H01X),
 C01L(H01Y,H,HA), C01M(H01Z,HB,HC), C01R(H01,HD,HE)
;
_shelx_res_checksum              25773
_shelx_hkl_checksum              70590
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.922
_oxdiff_exptl_absorpt_empirical_full_min 0.546