Structure, spectroscopy and reactivity of a mononuclear copper hydroxide complex in three molecular oxidation states.
Wu, Tong; MacMillan, Samantha N.; Rajabimoghadam, Khashayar; Siegler, Maxime A.; Lancaster, Kyle M.; Garcia-Bosch, Isaac; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c03867

data_4135100
_publ_section_title
;
 Structure, spectroscopy and reactivity of a mononuclear copper hydroxide
 complex in three molecular oxidation states.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c03867
_journal_year                    2020
_chemical_formula_moiety
'4(C22 H29 Cu N5 O3), 5(C3 H7 N O), 8(C4 H12 N)'
_chemical_formula_sum            'C135 H247 Cu4 N33 O17'
_chemical_formula_weight         2858.80
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 93.3428(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   61.4081(5)
_cell_length_b                   11.47738(11)
_cell_length_c                   22.2013(2)
_cell_measurement_reflns_used    55688
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      72.62
_cell_measurement_theta_min      2.47
_cell_volume                     15620.9(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_molecular_graphics    'SHELXTL v6.10 (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL v6.10 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, 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  0.0212
_diffrn_reflns_av_unetI/netI     0.0128
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       73
_diffrn_reflns_limit_h_min       -75
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            104531
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.900
_diffrn_reflns_theta_min         2.883
_exptl_absorpt_coefficient_mu    1.154
_exptl_absorpt_correction_T_max  0.855
_exptl_absorpt_correction_T_min  0.618
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29c (Rigaku Oxford Diffraction, 2017)
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-brown
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_description       block
_exptl_crystal_F_000             6160
_exptl_crystal_size_max          0.64
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.922
_refine_diff_density_min         -0.484
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     991
_refine_ls_number_reflns         15321
_refine_ls_number_restraints     219
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0424
_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^)+(0.0656P)^2^+26.2794P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1186
_refine_ls_wR_factor_ref         0.1193
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14935
_reflns_number_total             15321
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c03867_si_002.cif
_cod_data_source_block           tBuCuOH_NMe4_2
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4135100
_shelx_shelxl_version_number     2018/3
_oxdiff_exptl_absorpt_empirical_full_min 0.604
_oxdiff_exptl_absorpt_empirical_full_max 1.520
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              7430
_shelx_hkl_checksum              98496