Sub-nanometer Cu(i) clusters: coordination-modulated (Se vs. S) atom-packing mode and emission.
Ke, Feng; Song, Yongbo; Li, Hao; Zhou, Chuanjun; Du, Yuanxin; Zhu, Manzhou; Dalton transactions (Cambridge, England : 2003) 48 (2019) 13921–13924; doi:10.1039/c9dt02908g

data_7700942
_publ_section_title
;
 Sub-nanometer Cu(i) clusters: coordination-modulated (Se vs. S)
 atom-packing mode and emission.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13921
_journal_page_last               13924
_journal_paper_doi               10.1039/c9dt02908g
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety
'C150 H125 Cu13 P4 Se13, C H2 Cl2, 3[CH2Cl2], 2[CH2Cl2]'
_chemical_formula_sum            'C159 H143 Cl18 Cu13 P4 Se13'
_chemical_formula_weight         4668.21
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-07-25
_audit_creation_method
;
Olex2 1.3-dev
(compiled 2019.03.18 svn.r3573 for OlexSys, GUI svn.r5830)
;
_audit_update_record
;
2019-08-06 deposited with the CCDC.    2019-08-27 downloaded from the CCDC.
;
_cell_angle_alpha                79.2200(10)
_cell_angle_beta                 87.641(2)
_cell_angle_gamma                63.6130(10)
_cell_formula_units_Z            2
_cell_length_a                   17.6959(19)
_cell_length_b                   19.509(2)
_cell_length_c                   25.994(3)
_cell_measurement_reflns_used    9197
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.61
_cell_measurement_theta_min      2.18
_cell_volume                     7888.1(15)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.898
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0523
_diffrn_reflns_av_unetI/netI     0.1056
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.898
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            61767
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.898
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.140
_diffrn_reflns_theta_min         1.299
_exptl_absorpt_coefficient_mu    5.110
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5272
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1349 before and 0.0476 after correction.
The Ratio of minimum to maximum transmission is 0.7072.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.965
_exptl_crystal_description       cubic
_exptl_crystal_F_000             4564
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.076
_refine_diff_density_min         -1.045
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1648
_refine_ls_number_reflns         31370
_refine_ls_number_restraints     2106
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.1187
_refine_ls_R_factor_gt           0.0620
_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^)+(0.0858P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1522
_refine_ls_wR_factor_ref         0.1752
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17967
_reflns_number_total             31370
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02908g2.cif
_cod_data_source_block           aaa
_cod_depositor_comments          'Adding full bibliography for 7700942.cif.'
_cod_database_code               7700942
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Rigid bond restraints
 C8BA, C9CA, C0DA, C1DA, C2DA, C3DA, C0AA, C1AA, C2AA, C3AA, C4AA, C5AA, C6AA,
 C7AA, C8AA, C0BA, C1BA, C2BA, C4BA, C5BA, C6BA, C7BA, C9BA, C0CA, C1CA, C2CA,
 C3CA, C4CA, C5CA, C6CA, C8CA, C4DA, C5EA, C6FA, C7GA, C9GA, C0HA, C2HA, C3HA,
 C5DA, C6DA, C8DA, C9DA, C0EA, C1EA, C2EA, C3EA, C4EA, C6EA, C7EA, C8EA, C9EA,
 C0FA, C1FA, C2FA, C3FA, C4FA, C5FA, C7FA, C8FA, C9FA, C0GA, C1GA, C2GA, C3GA,
 C4GA, C5GA, C6GA, C8GA, C4HA, C5IA, C6JA, C7KA, C9KA, C0LA, C1LA, C2LA, C3LA,
 C5HA, C6HA, C7HA, C8HA, C9HA, C0IA, C1IA, C2IA, C3IA, C4IA, C6IA, C7IA, C8IA,
 C9IA, C0JA, C1JA, C2JA, C3JA, C4JA, C5JA, C8JA, C9JA, C0KA, C1KA, C2KA, C3KA,
 C4KA, C5KA, C6KA, C8KA, C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12, C14,
  C16, C17, C18, C19, C20, C21, C22, C23, C24, C25, C26, C27, C28, C29, C30,
 C31, C33, C34, C36, C37, C39, C6LA, C8LA, C0MA, C4LA, C5LA, C7LA, C9LA, C9AA,
 C3BA
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C8BA \\sim C9CA \\sim C0DA \\sim C1DA \\sim C2DA \\sim C3DA \\sim C0AA \\sim
C1AA \\sim C2AA \\sim C3AA \\sim C4AA \\sim C5AA \\sim C6AA \\sim C7AA \\sim
C8AA \\sim C0BA \\sim C1BA \\sim C2BA \\sim C4BA \\sim C5BA \\sim C6BA \\sim
C7BA \\sim C9BA \\sim C0CA \\sim C1CA \\sim C2CA \\sim C3CA \\sim C4CA \\sim
C5CA \\sim C6CA \\sim C8CA \\sim C4DA \\sim C5EA \\sim C6FA \\sim C7GA \\sim
C9GA \\sim C0HA \\sim C2HA \\sim C3HA \\sim C5DA \\sim C6DA \\sim C8DA \\sim
C9DA \\sim C0EA \\sim C1EA \\sim C2EA \\sim C3EA \\sim C4EA \\sim C6EA \\sim
C7EA \\sim C8EA \\sim C9EA \\sim C0FA \\sim C1FA \\sim C2FA \\sim C3FA \\sim
C4FA \\sim C5FA \\sim C7FA \\sim C8FA \\sim C9FA \\sim C0GA \\sim C1GA \\sim
C2GA \\sim C3GA \\sim C4GA \\sim C5GA \\sim C6GA \\sim C8GA \\sim C4HA \\sim
C5IA \\sim C6JA \\sim C7KA \\sim C9KA \\sim C0LA \\sim C1LA \\sim C2LA \\sim
C3LA \\sim C5HA \\sim C6HA \\sim C7HA \\sim C8HA \\sim C9HA \\sim C0IA \\sim
C1IA \\sim C2IA \\sim C3IA \\sim C4IA \\sim C6IA \\sim C7IA \\sim C8IA \\sim
C9IA \\sim C0JA \\sim C1JA \\sim C2JA \\sim C3JA \\sim C4JA \\sim C5JA \\sim
C8JA \\sim C9JA \\sim C0KA \\sim C1KA \\sim C2KA \\sim C3KA \\sim C4KA \\sim
C5KA \\sim C6KA \\sim C8KA \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim
C6 \\sim C7 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C14 \\sim C16
\\sim C17 \\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24
\\sim C25 \\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C33
\\sim C34 \\sim C36 \\sim C37 \\sim C39 \\sim C6LA \\sim C8LA \\sim C0MA \\sim
C4LA \\sim C5LA \\sim C7LA \\sim C9LA \\sim C9AA \\sim C3BA: within 2A with
sigma of 0.02 and sigma for terminal atoms of 0.01 within 2A
Uanis(C8BA) \\sim Ueq, Uanis(C9CA) \\sim Ueq, Uanis(C0DA) \\sim Ueq,
Uanis(C1DA) \\sim Ueq, Uanis(C2DA) \\sim Ueq, Uanis(C3DA) \\sim Ueq,
Uanis(C0AA) \\sim Ueq, Uanis(C1AA) \\sim Ueq, Uanis(C2AA) \\sim Ueq,
Uanis(C3AA) \\sim Ueq, Uanis(C4AA) \\sim Ueq, Uanis(C5AA) \\sim Ueq,
Uanis(C6AA) \\sim Ueq, Uanis(C7AA) \\sim Ueq, Uanis(C8AA) \\sim Ueq,
Uanis(C0BA) \\sim Ueq, Uanis(C1BA) \\sim Ueq, Uanis(C2BA) \\sim Ueq,
Uanis(C4BA) \\sim Ueq, Uanis(C5BA) \\sim Ueq, Uanis(C6BA) \\sim Ueq,
Uanis(C7BA) \\sim Ueq, Uanis(C9BA) \\sim Ueq, Uanis(C0CA) \\sim Ueq,
Uanis(C1CA) \\sim Ueq, Uanis(C2CA) \\sim Ueq, Uanis(C3CA) \\sim Ueq,
Uanis(C4CA) \\sim Ueq, Uanis(C5CA) \\sim Ueq, Uanis(C6CA) \\sim Ueq,
Uanis(C8CA) \\sim Ueq, Uanis(C4DA) \\sim Ueq, Uanis(C5EA) \\sim Ueq,
Uanis(C6FA) \\sim Ueq, Uanis(C7GA) \\sim Ueq, Uanis(C9GA) \\sim Ueq,
Uanis(C0HA) \\sim Ueq, Uanis(C2HA) \\sim Ueq, Uanis(C3HA) \\sim Ueq,
Uanis(C5DA) \\sim Ueq, Uanis(C6DA) \\sim Ueq, Uanis(C8DA) \\sim Ueq,
Uanis(C9DA) \\sim Ueq, Uanis(C0EA) \\sim Ueq, Uanis(C1EA) \\sim Ueq,
Uanis(C2EA) \\sim Ueq, Uanis(C3EA) \\sim Ueq, Uanis(C4EA) \\sim Ueq,
Uanis(C6EA) \\sim Ueq, Uanis(C7EA) \\sim Ueq, Uanis(C8EA) \\sim Ueq,
Uanis(C9EA) \\sim Ueq, Uanis(C0FA) \\sim Ueq, Uanis(C1FA) \\sim Ueq,
Uanis(C2FA) \\sim Ueq, Uanis(C3FA) \\sim Ueq, Uanis(C4FA) \\sim Ueq,
Uanis(C5FA) \\sim Ueq, Uanis(C7FA) \\sim Ueq, Uanis(C8FA) \\sim Ueq,
Uanis(C9FA) \\sim Ueq, Uanis(C0GA) \\sim Ueq, Uanis(C1GA) \\sim Ueq,
Uanis(C2GA) \\sim Ueq, Uanis(C3GA) \\sim Ueq, Uanis(C4GA) \\sim Ueq,
Uanis(C5GA) \\sim Ueq, Uanis(C6GA) \\sim Ueq, Uanis(C8GA) \\sim Ueq,
Uanis(C4HA) \\sim Ueq, Uanis(C5IA) \\sim Ueq, Uanis(C6JA) \\sim Ueq,
Uanis(C7KA) \\sim Ueq, Uanis(C9KA) \\sim Ueq, Uanis(C0LA) \\sim Ueq,
Uanis(C1LA) \\sim Ueq, Uanis(C2LA) \\sim Ueq, Uanis(C3LA) \\sim Ueq,
Uanis(C5HA) \\sim Ueq, Uanis(C6HA) \\sim Ueq, Uanis(C7HA) \\sim Ueq,
Uanis(C8HA) \\sim Ueq, Uanis(C9HA) \\sim Ueq, Uanis(C0IA) \\sim Ueq,
Uanis(C1IA) \\sim Ueq, Uanis(C2IA) \\sim Ueq, Uanis(C3IA) \\sim Ueq,
Uanis(C4IA) \\sim Ueq, Uanis(C6IA) \\sim Ueq, Uanis(C7IA) \\sim Ueq,
Uanis(C8IA) \\sim Ueq, Uanis(C9IA) \\sim Ueq, Uanis(C0JA) \\sim Ueq,
Uanis(C1JA) \\sim Ueq, Uanis(C2JA) \\sim Ueq, Uanis(C3JA) \\sim Ueq,
Uanis(C4JA) \\sim Ueq, Uanis(C5JA) \\sim Ueq, Uanis(C8JA) \\sim Ueq,
Uanis(C9JA) \\sim Ueq, Uanis(C0KA) \\sim Ueq, Uanis(C1KA) \\sim Ueq,
Uanis(C2KA) \\sim Ueq, Uanis(C3KA) \\sim Ueq, Uanis(C4KA) \\sim Ueq,
Uanis(C5KA) \\sim Ueq, Uanis(C6KA) \\sim Ueq, Uanis(C8KA) \\sim Ueq, Uanis(C1)
\\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq,
Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim
Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq,
Uanis(C12) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C17)
\\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C20) \\sim Ueq,
Uanis(C21) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C24)
\\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq,
Uanis(C28) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C31)
\\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C36) \\sim Ueq,
Uanis(C37) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C6LA) \\sim Ueq, Uanis(C8LA)
\\sim Ueq, Uanis(C0MA) \\sim Ueq, Uanis(C4LA) \\sim Ueq, Uanis(C5LA) \\sim Ueq,
Uanis(C7LA) \\sim Ueq, Uanis(C9LA) \\sim Ueq, Uanis(C9AA) \\sim Ueq,
Uanis(C3BA) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.01
4.a Secondary CH2 refined with riding coordinates:
 C3BA(H3BA,H3BB)
4.b Aromatic/amide H refined with riding coordinates:
 C3DA(H3DA), C0AA(H0AA), C2AA(H2AA), C7AA(H7AA), C8AA(H8AA), C2BA(H2BA),
 C5BA(H5BA), C6BA(H6BA), C7BA(H7BA), C0CA(H0CA), C1CA(H1CA), C3CA(H3CA),
 C8CA(H8CA), C4DA(H4DA), C5EA(H5EA), C6FA(H6FA), C9GA(H9GA), C2HA(H2HA),
 C3HA(H3HA), C5DA(H5DA), C6DA(H6DA), C8DA(H8DA), C9DA(H9DA), C0EA(H0EA),
 C1EA(H1EA), C2EA(H2EA), C3EA(H3EA), C4EA(H4EA), C6EA(H6EA), C7EA(H7EA),
 C8EA(H8EA), C9EA(H9EA), C0FA(H0FA), C1FA(H1FA), C2FA(H2FA), C3FA(H3FA),
 C4FA(H4FA), C5FA(H5FA), C7FA(H7FA), C8FA(H8FA), C9FA(H9FA), C0GA(H0GA),
 C1GA(H1GA), C2GA(H2GA), C3GA(H3GA), C4GA(H4GA), C5GA(H5GA), C6GA(H6GA),
 C8GA(H8GA), C5IA(H5IA), C6JA(H6JA), C7KA(H7KA), C0LA(H0LA), C1LA(H1LA),
 C3LA(H3LA), C5HA(H5HA), C6HA(H6HA), C7HA(H7HA), C8HA(H8HA), C9HA(H9HA),
 C0IA(H0IA), C1IA(H1IA), C2IA(H2IA), C3IA(H3IA), C6IA(H6IA), C8IA(H8IA),
 C9IA(H9IA), C0JA(H0JA), C1JA(H1JA), C2JA(H2JA), C3JA(H3JA), C4JA(H4JA),
 C5JA(H5JA), C8JA(H8JA), C9JA(H9JA), C0KA(H0KA), C1KA(H1KA), C2KA(H2KA),
 C3KA(H3KA), C4KA(H4KA), C5KA(H5KA), C6KA(H6KA), C8KA(H8KA), C1(H1), C2(H2),
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21),
  C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28),
 C29(H29), C30(H30), C31(H31), C33(H33), C34(H34), C36(H36), C37(H37), C39(H39),
  C6LA(H6LA), C8LA(H8LA), C0MA(H0MA), C4LA(H4LA), C5LA(H5LA), C7LA(H7LA),
 C9LA(H9LA), C9AA(H9AA)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 455 electrons were
found in a volume of 1253\%A^3 in 2 voids per unit cell.
This is consistent with the presence of 3[CH2Cl2] in one
void and then another 2[CH2Cl2] in another void per Formula
Unit, which accounts for 420 electrons per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              99261
_shelx_fab_checksum              90045
_olex2_submission_special_instructions 'No special instructions were received'