Luminescence Solvato- and Vapochromism of Alkynyl-Phosphine Copper Clusters.
Krytchankou, Ilya S.; Koshevoy, Igor O.; Gurzhiy, Vladislav V.; Pomogaev, Vladimir A.; Tunik, Sergey P.; Inorganic chemistry 54 (2015) 8288–8297; doi:10.1021/acs.inorgchem.5b00239

data_4346079
_publ_section_title
;
 Luminescence Solvato- and Vapochromism of Alkynyl-Phosphine Copper
 Clusters.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8288
_journal_page_last               8297
_journal_paper_doi               10.1021/acs.inorgchem.5b00239
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety
'C51 H39 Cu3 N2 P3, F6 P, 0.4(C4 H8 O), C2 H3 N'
_chemical_formula_sum            'C54.6 H45.2 Cu3 F6 N3 O0.4 P4'
_chemical_formula_weight         1178.23
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-07-04
_audit_creation_method
;
Olex2 1.2
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846)
;
_cell_angle_alpha                98.586(3)
_cell_angle_beta                 105.357(3)
_cell_angle_gamma                92.078(4)
_cell_formula_units_Z            2
_cell_length_a                   11.9838(5)
_cell_length_b                   14.5634(7)
_cell_length_c                   15.0567(4)
_cell_measurement_reflns_used    5722
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.6410
_cell_measurement_theta_min      2.9520
_cell_volume                     2497.62(18)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.2096
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
  1 omega  -25.00   24.00   1.0000  140.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.8777  -99.0000  120.0000 49

  2 omega  -82.00  -54.00   1.0000  140.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.8777 -168.0000    4.0000 28

  3 omega  -23.00    7.00   1.0000  140.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.8777  -99.0000    0.0000 30

  4 omega   35.00   95.00   1.0000  140.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8152  178.0000 -180.0000 60

  5 omega    0.00   88.00   1.0000  140.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8152   57.0000  -90.0000 88

  6 omega   51.00   77.00   1.0000  140.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8152 -178.0000   90.0000 26

  7 omega   -6.00   88.00   1.0000  140.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8152   38.0000    0.0000 94

  8 omega  -43.00   28.00   1.0000  140.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8152  -19.0000  150.0000 71
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0275445000
_diffrn_orient_matrix_UB_12      -0.0020507000
_diffrn_orient_matrix_UB_13      0.0474844000
_diffrn_orient_matrix_UB_21      -0.0033796000
_diffrn_orient_matrix_UB_22      0.0486471000
_diffrn_orient_matrix_UB_23      0.0116653000
_diffrn_orient_matrix_UB_31      -0.0549662000
_diffrn_orient_matrix_UB_32      -0.0084192000
_diffrn_orient_matrix_UB_33      0.0079035000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_av_unetI/netI     0.1158
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22753
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.491
_diffrn_reflns_theta_min         2.554
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.459
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94128
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow-green
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_description       prism
_exptl_crystal_F_000             1196
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.867
_refine_diff_density_min         -1.010
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     632
_refine_ls_number_reflns         11067
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0970
_refine_ls_R_factor_gt           0.0598
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0247P)^2^+2.3970P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1069
_refine_ls_wR_factor_ref         0.1272
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7639
_reflns_number_total             11067
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00239_si_003.cif
_cod_data_source_block           6b
_cod_original_cell_volume        2497.62(19)
_cod_original_formula_sum        'C54.60 H45.20 Cu3 F6 N3 O0.40 P4'
_cod_database_code               4346079
_shelxl_version_number           2013-4
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Restrained distances
 P4-F4A = P4-F5A = P4-F6A = P4-F3B = P4-F1 = P4-F2A = P4-F2B = P4-F5B = P4-F4B
 = P4-F3A = P4-F6B
 1.75 with sigma of 0.02
 C55A_$1-C54A_$1 = C55B_$1-C54B_$1
 1.45 with sigma of 0.02
 C54B-C55B = C55A-C54A
 1.45 with sigma of 0.02
 O1-C55B
 1.45 with sigma of 0.02
 C55A-O1
 1.45 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F4A) = Uanis(F5A) = Uanis(F6A) = Uanis(F3B) = Uanis(F1) = Uanis(F2A) =
Uanis(F2B) = Uanis(F5B) = Uanis(F4B) = Uanis(F3A) = Uanis(F6B)
Uanis(O1) = Uanis(C55A) = Uanis(C54B) = Uanis(C55A) = Uanis(C54B)
Uanis(C54B) = Uanis(O1) = Uanis(C55A) = Uanis(C55B) = Uanis(C54A)
4. Others
 Sof(F3B)=Sof(F6B)=Sof(F5B)=Sof(F2B)=Sof(F4B)=1-FVAR(1)
 Sof(F2A)=Sof(F3A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=FVAR(1)
 Fixed Sof: O1(0.4) C54B(0.4) H54A(0.4) H54B(0.4) H54C(0.4) C55B(0.4)
 C54A(0.4) H54D(0.4) H54E(0.4) H54F(0.4) C55A(0.4) H55A(0.4) H55B(0.4)
5.a Ternary CH refined with riding coordinates:
 C1(H1)
5.b Secondary CH2 refined with riding coordinates:
 C55A(H55A,H55B)
5.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13), C14(H14), C15(H15),
 C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C23(H23), C24(H24), C25(H25),
  C26(H26), C27(H27), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33),
 C35(H35), C36(H36), C37(H37), C38(H38), C39(H39), C41(H41), C42(H42), C43(H43),
  C44(H44), C45(H45), C47(H47), C48(H48), C49(H49), C50(H50), C51(H51)
5.d Idealised Me refined as rotating group:
 C54B(H54A,H54B,H54C), C54A(H54D,H54E,H54F), C53(H53A,H53B,H53C)
;