Isolation of an unusual [Cu6] nanocluster through sequential addition of copper(i) to a polynucleating ligand.
Phanopoulos, Andreas; Warren, Mark; White, Andrew J. P.; Horton, Andrew; Crimmin, Mark R.; Dalton transactions (Cambridge, England : 2003) 46 (2017) 2077–2080; doi:10.1039/c6dt04703c

data_7041767
_publ_section_title
;
 Isolation of an unusual [Cu6] nanocluster through sequential addition of
 copper(i) to a polynucleating ligand.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2077
_journal_page_last               2080
_journal_paper_doi               10.1039/c6dt04703c
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C78 H102 Cu6 I2 N10, 1.5(C4 H10 O)'
_chemical_formula_sum            'C84 H117 Cu6 I2 N10 O1.5'
_chemical_formula_weight         1925.91
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-08-24 deposited with the CCDC.
2017-01-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.7700(5)
_cell_length_b                   15.1245(3)
_cell_length_c                   22.5140(4)
_cell_measurement_reflns_used    8257
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.2980
_cell_measurement_theta_min      2.6420
_cell_volume                     9115.5(3)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 16.0382
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.807
_diffrn_measurement_device_type  'Agilent Xcalibur 3 E'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0213
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.807
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20020
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.807
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.328
_diffrn_reflns_theta_min         2.721
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.099
_exptl_absorpt_correction_T_max  0.665
_exptl_absorpt_correction_T_min  0.621
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) 
(compiled Aug 13 2014,18:06:01) 
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            'Dark orange'
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_description       blocks
_exptl_crystal_F_000             3932
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.864
_refine_diff_density_min         -0.809
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.072(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     978
_refine_ls_number_reflns         13046
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0345
_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^)+(0.0413P)^2^+4.7541P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0789
_refine_ls_wR_factor_ref         0.0854
_reflns_Friedel_coverage         0.949
_reflns_Friedel_fraction_full    0.990
_reflns_Friedel_fraction_max     0.806
_reflns_number_gt                11563
_reflns_number_total             13046
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04703c2.cif
_cod_data_source_block           LCu3I_2-I
_cod_depositor_comments
'Adding full bibliography for 7041766--7041768.cif.'
_cod_original_cell_volume        9115.6(3)
_cod_original_formula_sum        'C84 H117 Cu6 I2 N10 O1.50'
_cod_database_code               7041767
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              32528