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_7041768
_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 Cu4 N10, 2(C4 H10 O)'
_chemical_formula_sum            'C86 H122 Cu4 N10 O2'
_chemical_formula_weight         1582.18
_chemical_name_systematic        'Cu4 cluster'
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-01-13
_audit_creation_method
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Olex2 1.2
(compiled Dec 12 2016 15:38:10 for OlexSys, GUI svn.r5292)
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_audit_update_record
;
2017-01-14 deposited with the CCDC.
2017-01-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.596(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.8050(6)
_cell_length_b                   11.3607(4)
_cell_length_c                   27.7024(7)
_cell_measurement_reflns_used    14413
_cell_measurement_temperature    300
_cell_measurement_theta_max      25.5430
_cell_measurement_theta_min      1.8910
_cell_volume                     8341.3(4)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      300
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.9574
_diffrn_measured_fraction_theta_max 0.9574
_diffrn_measurement_details
;
  1 omega  -90.00   38.00   0.4000    0.3970
omega____ theta____ kappa____ phi______ frames
    -       30.0000   65.0000  -80.0000 320

  2 phi    -80.00   40.00   0.4000    0.3970
omega____ theta____ kappa____ phi______ frames
  38.0000   30.0000   65.0000     -     300

  3 omega  -90.00   38.00   0.4000    0.3970
omega____ theta____ kappa____ phi______ frames
    -       30.0000   65.0000   40.0000 320

  4 phi     40.00  160.00   0.4000    0.3970
omega____ theta____ kappa____ phi______ frames
  38.0000   30.0000   65.0000     -     300

  5 omega  -90.00   38.00   0.4000    0.3970
omega____ theta____ kappa____ phi______ frames
    -       30.0000   65.0000  160.0000 320

  6 phi    -90.00  150.00   0.4000    0.3970
omega____ theta____ kappa____ phi______ frames
  38.0000   30.0000    0.0000     -     600
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'dectris-CrysAlisPro-abstract goniometer imported dectris images'
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_diffrn_orient_matrix_UB_21      -0.0049732000
_diffrn_orient_matrix_UB_22      -0.0078705000
_diffrn_orient_matrix_UB_23      -0.0249152000
_diffrn_orient_matrix_UB_31      0.0034329000
_diffrn_orient_matrix_UB_32      -0.0597459000
_diffrn_orient_matrix_UB_33      0.0031120000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0841
_diffrn_reflns_av_unetI/netI     0.0752
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            76322
_diffrn_reflns_theta_full        25.5032
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.72
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.972
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54661
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.2598
_exptl_crystal_description       needle
_exptl_crystal_F_000             3365.9718
_exptl_crystal_recrystallization_method 'from diethylether'
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.004
_exptl_crystal_size_min          0.004
_refine_diff_density_max         0.7885
_refine_diff_density_min         -0.9547
_refine_diff_density_rms         0.1484
_refine_ls_d_res_high            0.8000
_refine_ls_d_res_low             11.4871
_refine_ls_goodness_of_fit_ref   1.0086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    190
_refine_ls_number_parameters     959
_refine_ls_number_reflns         16339
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0086
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_gt           0.0515
_refine_ls_shift/su_max          0.0002
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0687P)^2^+1.9450P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1176
_refine_ls_wR_factor_ref         0.1333
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              33
_reflns_limit_h_min              -33
_reflns_limit_k_max              14
_reflns_limit_k_min              0
_reflns_limit_l_max              34
_reflns_limit_l_min              0
_reflns_number_gt                11244
_reflns_number_total             16339
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c6dt04703c2.cif
_cod_data_source_block           AP001_Et2O_03_0
_cod_depositor_comments
'Adding full bibliography for 7041766--7041768.cif.'
_cod_database_code               7041768
_chemical_oxdiff_formula         'C39 H51 N5 Cu2'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: O2(0.6) C83(0.6) H83a(0.6) H83b(0.6) C84(0.6) H84a(0.6) H84b(0.6)
 C85(0.6) H85a(0.6) H85b(0.6) H85c(0.6) C86(0.6) H86a(0.6) H86b(0.6) H86c(0.6)
 C1A(0.4) H1Aa(0.4) H1Ab(0.4) C1B(0.4) H1Ba(0.4) H1Bb(0.4) O2B(0.4) C1C(0.4)
 H1Ca(0.4) H1Cb(0.4) H1Cc(0.4) C1D(0.4) H1Da(0.4) H1Db(0.4) H1Dc(0.4)
3.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C34(H34), C37(H37), C46(H46), C49(H49), C73(H73), C76(H76)
3.b Secondary CH2 refined with riding coordinates:
 C79(H79a,H79b), C81(H81a,H81b), C83(H83a,H83b), C84(H84a,H84b), C1A(H1Aa,
 H1Ab), C1B(H1Ba,H1Bb)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C14(H14), C19(H19), C24(H24), C30(H30), C31(H31),
 C32(H32), C42(H42), C43(H43), C44(H44), C53(H53), C60(H60), C63(H63), C69(H69),
  C70(H70), C71(H71)
3.d Idealised Me refined as rotating group:
 C8(H8a,H8b,H8c), C9(H9a,H9b,H9c), C11(H11a,H11b,H11c), C12(H12a,H12b,H12c),
 C16(H16a,H16b,H16c), C17(H17a,H17b,H17c), C26(H26a,H26b,H26c), C27(H27a,H27b,
 H27c), C35(H35a,H35b,H35c), C36(H36a,H36b,H36c), C38(H38a,H38b,H38c), C39(H39a,
 H39b,H39c), C47(H47a,H47b,H47c), C48(H48a,H48b,H48c), C50(H50a,H50b,H50c),
 C51(H51a,H51b,H51c), C55(H55a,H55b,H55c), C56(H56a,H56b,H56c), C65(H65a,H65b,
 H65c), C66(H66a,H66b,H66c), C74(H74a,H74b,H74c), C75(H75a,H75b,H75c), C77(H77a,
 H77b,H77c), C78(H78a,H78b,H78c), C80(H80a,H80b,H80c), C82(H82a,H82b,H82c),
 C85(H85a,H85b,H85c), C86(H86a,H86b,H86c), C1C(H1Ca,H1Cb,H1Cc), C1D(H1Da,H1Db,
 H1Dc)
;
_olex2_submission_original_sample_id AP001
_olex2_submission_special_instructions 'No special instructions were received'