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_4347035
_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         'C68 H64 Cu3 I2 N2 P6, B F4, C2 H3 N'
_chemical_formula_sum            'C70 H67 B Cu3 F4 I2 N3 P6'
_chemical_formula_weight         1667.31
_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             2015-12-21
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                94.291(2)
_cell_angle_beta                 107.910(2)
_cell_angle_gamma                102.175(2)
_cell_formula_units_Z            2
_cell_length_a                   14.1918(2)
_cell_length_b                   15.0336(3)
_cell_length_c                   21.1593(4)
_cell_measurement_reflns_used    24455
_cell_measurement_temperature    122.97(19)
_cell_measurement_theta_max      70.6358
_cell_measurement_theta_min      3.0391
_cell_volume                     4151.42(15)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      122.97(19)
_diffrn_detector_area_resol_mean 10.3546
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_details
;
  1 omega  -97.00   -3.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.2064  125.0000  -30.0000 188

  2 omega   15.00  108.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       41.2064   37.0000  -30.0000 186

  3 omega  -31.00   67.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       41.2064  -37.0000  150.0000 196

  4 omega  -44.00   -4.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000   77.0000  120.0000 80

  5 omega   23.00   69.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      100.5179  -30.0000  120.0000 92

  6 omega   24.00  132.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      100.5179  -77.0000  -60.0000 216

  7 omega   24.00   68.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      100.5179  -30.0000  -30.0000 88

  8 omega   42.00  152.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      100.5179   15.0000  -60.0000 220

  9 omega   71.00  154.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      100.5179   61.0000  120.0000 166

 10 omega   27.00   68.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      100.5179  -30.0000  -60.0000 82

 11 omega   48.00  134.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      100.5179  -77.0000  120.0000 172

 12 omega   26.00  122.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      100.5179 -125.0000  120.0000 192

 13 omega   37.00  108.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      100.5179  -94.0000  -90.0000 142

 14 omega    8.00  120.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       41.2064   77.0000  -30.0000 224

 15 omega   12.00  115.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       41.2064   57.0000 -150.0000 206

 16 omega   12.00  115.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       41.2064   57.0000   90.0000 206

 17 omega   70.00  158.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      100.5179   61.0000 -180.0000 176

 18 omega   73.00  158.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      100.5179   45.0000    0.0000 170

 19 omega   26.00   77.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      100.5179  -45.0000 -150.0000 102

 20 omega   26.00   77.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      100.5179  -45.0000   30.0000 102

 21 omega   70.00  158.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      100.5179   61.0000  -60.0000 176

 22 omega   70.00  133.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      100.5179   61.0000   90.0000 126

 23 omega   73.00  158.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      100.5179   45.0000   60.0000 170
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0589682000
_diffrn_orient_matrix_UB_12      -0.0402681000
_diffrn_orient_matrix_UB_13      -0.0743033000
_diffrn_orient_matrix_UB_21      -0.0957934000
_diffrn_orient_matrix_UB_22      -0.0397909000
_diffrn_orient_matrix_UB_23      0.0183541000
_diffrn_orient_matrix_UB_31      -0.0346807000
_diffrn_orient_matrix_UB_32      0.0896583000
_diffrn_orient_matrix_UB_33      -0.0114814000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            15495
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.680
_diffrn_reflns_theta_max         70.767
_diffrn_reflns_theta_min         3.042
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.189
_exptl_absorpt_correction_T_max  0.688
_exptl_absorpt_correction_T_min  0.349
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
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)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_description
;
;
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.2046
_exptl_crystal_size_mid          0.0761
_exptl_crystal_size_min          0.0578
_platon_squeeze_details
;
The electron count roughly corresponds to five tetrahydrofurane molecules
and one acetonitrile molecule. 
;
_refine_diff_density_max         1.843
_refine_diff_density_min         -0.861
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     807
_refine_ls_number_reflns         15495
_refine_ls_number_restraints     83
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0368
_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^)+(0.0692P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0968
_refine_ls_wR_factor_ref         0.1026
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12773
_reflns_number_total             15495
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02641_si_011.cif
_cod_data_source_block           sq
_cod_original_cell_volume        4151.42(14)
_cod_database_code               4347035
_chemical_oxdiff_formula         Cu3I2(P3C32H29)2(C2H3N)3.5(C4H8O)2.5B1F4
_reflns_odcompleteness_completeness 99.62
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_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
 B1-F1 \\sim B1-F2 \\sim B1-F3 \\sim B1-F4 \\sim B2-F5 \\sim B2-F6 \\sim B2-F7
\\sim B2-F8
 with sigma of 0.02
 F1-F2 \\sim F1-F3 \\sim F1-F4 \\sim F2-F3 \\sim F2-F4 \\sim F3-F4 \\sim F5-F6
\\sim F5-F7 \\sim F5-F8 \\sim F6-F7
 \\sim F6-F8
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uiso(F5) = Uiso(F6) = Uiso(F7) = Uiso(F8)
4. Others
 Fixed Sof: C2(0.5) H2A(0.5) H2B(0.5) H2C(0.5) B1(0.68) F1(0.68) F2(0.68)
 F3(0.68) F4(0.68) B2(0.32) F5(0.32) F6(0.32) F7(0.32) F8(0.32) C202(0.5)
 H20A(0.5) H20B(0.5) H20C(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B)
5.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C16(H16), C17(H17),
 C18(H18), C19(H19), C20(H20), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26),
  C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C34(H34), C35(H35),
 C36(H36), C37(H37), C38(H38), C40(H40), C41(H41), C42(H42), C43(H43), C44(H44),
  C46(H46), C47(H47), C48(H48), C49(H49), C50(H50), C52(H52), C53(H53),
 C54(H54), C55(H55), C56(H56), C58(H58), C59(H59), C60(H60), C61(H61), C62(H62),
  C64(H64), C65(H65), C66(H66), C67(H67), C68(H68)
5.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C901(H90A,H90B,H90C), C202(H20A,H20B,H20C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'