Self-Assembly of Reactive Linear Cu3 Building Blocks for Supramolecular Coordination Chemistry and Their Reactivity toward E(n) Ligand Complexes.
Fleischmann, Martin; Dütsch, Luis; Elsayed Moussa, Mehdi; Balázs, Gábor; Kremer, Werner; Lescop, Christophe; Scheer, Manfred; Inorganic chemistry 55 (2016) 2840–2854; doi:10.1021/acs.inorgchem.5b02641

data_4347038
_publ_section_title
;
 Self-Assembly of Reactive Linear Cu3 Building Blocks for Supramolecular
 Coordination Chemistry and Their Reactivity toward E(n) Ligand Complexes.
;
_journal_issue                   6
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2840
_journal_page_last               2854
_journal_paper_doi               10.1021/acs.inorgchem.5b02641
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C64 H58 Cu3 I2 P6, B F4, 2(C H2 Cl2)'
_chemical_formula_sum            'C66 H62 B Cl4 Cu3 F4 I2 P6'
_chemical_formula_weight         1714.00
_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             2015-08-11
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                95.7164(11)
_cell_angle_beta                 106.7947(13)
_cell_angle_gamma                101.5198(12)
_cell_formula_units_Z            2
_cell_length_a                   14.1533(2)
_cell_length_b                   15.0547(2)
_cell_length_c                   21.4267(3)
_cell_measurement_reflns_used    22240
_cell_measurement_temperature    122.9(6)
_cell_measurement_theta_max      65.7610
_cell_measurement_theta_min      3.9280
_cell_volume                     4222.04(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      122.9(6)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2548
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
  1 omega  -26.00   57.00   0.5000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       39.9038  -57.0000  -90.0000 166

  2 omega    9.00  112.00   0.5000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       39.9038   57.0000   60.0000 206

  3 omega   51.00   77.00   0.5000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       39.9038 -125.0000 -150.0000 52

  4 omega   11.00   37.00   0.5000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       39.9038 -125.0000  -60.0000 52

  5 omega    9.00   94.00   0.5000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       39.9038   57.0000 -180.0000 170

  6 omega -123.00  -74.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -90.0000  127.0000  -74.1514 98

  7 omega -157.00 -130.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -90.0000  178.0000  -60.0000 54

  8 omega -154.00 -129.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -90.0000  178.0000 -180.0000 50

  9 omega   99.00  125.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -92.0000   97.8272 52

 10 omega   13.00   50.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -77.0000  -60.0000 74

 11 omega   94.00  120.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -91.0000  -98.2874 52

 12 omega   53.00   90.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -77.0000  -60.0000 74

 13 omega   32.00   67.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -94.0000 -180.0000 70

 14 omega  126.00  169.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   61.0000  150.0000 86

 15 omega   69.00  134.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000  140.7834 130

 16 omega  108.00  133.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -89.0000   48.5951 50

 17 omega   18.00   76.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000  120.0000 116

 18 omega    9.00   77.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -89.0000   48.5951 136

 19 omega   94.00  122.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000   24.2304 56

 20 omega   80.00  131.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  111.0000 -180.0000 102

 21 omega  142.00  167.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  111.0000 -180.0000 50

 22 omega    9.00   35.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -94.0000  -60.0000 52

 23 omega   54.00   80.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -94.0000  -60.0000 52

 24 omega   68.00  114.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000 -120.0000 92

 25 omega  103.00  129.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  111.0000  -90.0000 52

 26 omega  130.00  156.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  111.0000  -90.0000 52

 27 omega   85.00  113.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -61.0000   60.0000 56

 28 omega   62.00   89.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   61.0000  150.0000 54

 29 omega   34.00   61.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -30.0000  -90.0000 54

 30 omega   76.00  101.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   30.0000 -120.0000 50

 31 omega   16.00   67.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -30.0000   30.0000 102

 32 omega   55.00  147.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -17.0000   58.4507 184

 33 omega   43.00   69.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -94.0000   90.0000 52

 34 omega   72.00  108.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -90.0000  -41.3476 72

 35 omega    9.00   35.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -15.0000  -60.0000 52

 36 omega   57.00   82.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -15.0000  -60.0000 50

 37 omega  112.00  171.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -15.0000  -60.0000 118

 38 omega   40.00   76.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000  -90.0000 72

 39 omega  106.00  132.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  111.0000  -30.0000 52

 40 omega  148.00  173.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  111.0000  -30.0000 50

 41 omega   46.00   72.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000  150.0000 52

 42 omega   84.00  110.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   45.0000  -60.0000 52

 43 omega  124.00  163.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   45.0000  -60.0000 78

 44 omega   37.00   62.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -94.0000  -90.0000 50

 45 omega   20.00   45.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000 -111.0000 -150.0000 50

 46 omega   61.00   87.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000 -111.0000 -150.0000 52

 47 omega   92.00  117.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  178.0000  120.0000 50

 48 omega   31.00   56.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000 -180.0000 50

 49 omega   39.00   64.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000   60.0000 50

 50 omega    8.00   83.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -91.0000  -81.4043 150

 51 omega   12.00   37.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -90.0000  -41.3476 50

 52 omega   42.00   91.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  178.0000  -30.0000 98

 53 omega   33.00  125.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -86.0000   -5.5882 184

 54 omega   39.00   64.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -61.0000   60.0000 50

 55 omega   45.00   71.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000   24.2304 52

 56 omega   31.00   56.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -77.0000  150.0000 50

 57 omega   24.00   60.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000  140.7834 72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0277542000
_diffrn_orient_matrix_UB_12      0.0060699000
_diffrn_orient_matrix_UB_13      -0.0742100000
_diffrn_orient_matrix_UB_21      0.0060464000
_diffrn_orient_matrix_UB_22      -0.1004736000
_diffrn_orient_matrix_UB_23      -0.0154652000
_diffrn_orient_matrix_UB_31      -0.1136197000
_diffrn_orient_matrix_UB_32      -0.0330209000
_diffrn_orient_matrix_UB_33      -0.0075693000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_av_unetI/netI     0.0506
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            14597
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        65.990
_diffrn_reflns_theta_max         65.990
_diffrn_reflns_theta_min         3.360
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.193
_exptl_absorpt_correction_T_max  0.588
_exptl_absorpt_correction_T_min  0.216
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_description       block
_exptl_crystal_F_000             1700
_exptl_crystal_preparation
'recrystallization of [Cu3I2(dpmp)2][BF4] from cool CH2Cl2'
_exptl_crystal_size_max          0.2537
_exptl_crystal_size_mid          0.1181
_exptl_crystal_size_min          0.0598
_platon_squeeze_details
;
The solvent accessible void contains 9 to 10 dissordered CH2Cl2
solvent molecules.
;
_refine_diff_density_max         2.411
_refine_diff_density_min         -1.092
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.956
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     788
_refine_ls_number_reflns         14597
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      0.955
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_gt           0.0553
_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^)+(0.1117P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1451
_refine_ls_wR_factor_ref         0.1504
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11183
_reflns_number_total             14597
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02641_si_007.cif
_cod_data_source_block           cu3i2_dcm_sq_d
_cod_original_cell_volume        4222.06(11)
_cod_database_code               4347038
_chemical_oxdiff_formula         Cu3I2(P3C32H29)2(CH2Cl2)4(BF4)
_reflns_odcompleteness_completeness 96.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Cl4-C66 \\sim Cl5-C67
 with sigma of 0.02
 Cl3-C66 \\sim Cl3-C67
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C66) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.1
4. Others
 Fixed Sof: Cl4(0.75) C66(0.75) H66A(0.75) H66B(0.75) Cl5(0.25) C67(0.25)
 H67A(0.25) H67B(0.25)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C65(H65A,H65B), C66(H66A,
 H66B), C67(H67A,H67B)
5.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24),
  C25(H25), C26(H26), C27(H27), C28(H28), C30(H30), C31(H31), C32(H32),
 C33(H33), C34(H34), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C42(H42),
  C43(H43), C44(H44), C45(H45), C46(H46), C48(H48), C49(H49), C50(H50),
 C51(H51), C52(H52), C54(H54), C55(H55), C56(H56), C57(H57), C58(H58), C60(H60),
  C61(H61), C62(H62), C63(H63), C64(H64)
;
_shelx_shelxl_version_number     2014/7
_olex2_exptl_crystal_mounting_method 'cooled mineral oil'
_olex2_submission_original_sample_id Cu3I2_DCM
_olex2_submission_special_instructions 'No special instructions were received'