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_4347037
_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 Br2 Cu3 N2 P6, 0.68(C4 H10 O), B F4, 0.32(C4 H8 O)'
_chemical_formula_sum            'C72 H73.36 B Br2 Cu3 F4 N2 O P6'
_chemical_formula_weight         1605.75
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2015-06-24
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                88.2465(11)
_cell_angle_beta                 73.3789(11)
_cell_angle_gamma                77.9023(14)
_cell_formula_units_Z            2
_cell_length_a                   12.9373(2)
_cell_length_b                   13.4542(2)
_cell_length_c                   21.4483(2)
_cell_measurement_reflns_used    23111
_cell_measurement_temperature    122.9(4)
_cell_measurement_theta_max      65.8000
_cell_measurement_theta_min      4.4090
_cell_volume                     3496.16(9)
_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)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      122.9(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2548
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
  1 omega  -11.00  116.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       40.2788   19.0000    0.0000 254

  2 omega  118.00  171.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   30.0000  -90.0000 106

  3 omega  114.00  170.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   61.0000 -150.0000 112

  4 omega  114.00  156.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000    0.0000 -180.0000 84

  5 omega  103.00  131.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   30.0000 -150.0000 56

  6 omega   79.00  121.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  111.0000  -90.0000 84

  7 omega   67.00   93.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   30.0000 -150.0000 52

  8 omega   59.00   85.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000  -90.0000 52

  9 omega   32.00   82.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   10.0000   41.0528 100

 10 omega   87.00  129.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   30.0000   60.0000 84

 11 omega  101.00  149.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   10.0000   41.0528 96

 12 omega   94.00  170.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   45.0000  150.0000 152

 13 omega   87.00  112.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -61.0000   60.0000 50

 14 omega   78.00  104.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -92.0000   61.6454 52

 15 omega   91.00  127.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -77.0000    0.0000 72

 16 omega   94.00  120.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -92.0000  -47.7127 52

 17 omega   88.00  128.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000  -80.7809 80

 18 omega   52.00   78.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000 -111.0000 -150.0000 52

 19 omega   54.00   84.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -95.0000 -120.0000 60

 20 omega   43.00   79.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -92.0000  -47.7127 72

 21 omega   41.00   67.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000  -80.7809 52

 22 omega   34.00   59.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -61.0000  -60.0000 50

 23 omega   25.00   59.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -95.0000  -60.0000 68

 24 omega   26.00   94.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -61.0000    0.0000 136

 25 omega   57.00  107.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -91.0000   89.9037 100

 26 omega   83.00  133.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000  175.8478 100

 27 omega   57.00   83.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -61.0000  150.0000 52

 28 omega   41.00   67.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -95.0000   90.0000 52

 29 omega   37.00   62.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -92.0000   61.6454 50

 30 omega   32.00   68.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000   90.0000 72

 31 omega   34.00   59.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000 -111.0000  120.0000 50

 32 omega   27.00   77.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000  150.0000 100

 33 omega   13.00  114.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       40.2788   38.0000   60.0000 202

 34 omega   18.00   64.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -30.0000    0.0000 92

 35 omega   20.00   73.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000  -90.0000 106

 36 omega   25.00   67.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000 -150.0000 84

 37 omega   20.00   58.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000 -180.0000 76

 38 omega   18.00   47.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -95.0000 -180.0000 58

 39 omega   11.00   36.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -95.0000 -120.0000 50

 40 omega    8.00   36.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000  -80.7809 56

 41 omega   12.00   74.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -77.0000    0.0000 124

 42 omega   16.00  101.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -77.0000  120.0000 170

 43 omega   15.00   60.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -95.0000  120.0000 90

 44 omega   16.00   41.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -30.0000 -150.0000 50

 45 omega  -87.00  -61.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.2788  125.0000 -180.0000 52

 46 omega  105.00  134.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  178.0000   90.0000 58

 47 omega  -50.00  -24.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.2788  125.0000 -180.0000 52

 48 omega -120.00  -94.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -90.0000  132.0000  -92.1186 52

 49 omega -156.00 -121.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -90.0000  178.0000    0.0000 70

 50 omega  -91.00  -23.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.2788  125.0000   90.0000 136

 51 omega -156.00 -131.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -90.0000  178.0000 -120.0000 50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0689893000
_diffrn_orient_matrix_UB_12      -0.0998286000
_diffrn_orient_matrix_UB_13      -0.0364076000
_diffrn_orient_matrix_UB_21      0.1063225000
_diffrn_orient_matrix_UB_22      0.0306828000
_diffrn_orient_matrix_UB_23      0.0037994000
_diffrn_orient_matrix_UB_31      -0.0094624000
_diffrn_orient_matrix_UB_32      -0.0531030000
_diffrn_orient_matrix_UB_33      0.0654550000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0462
_diffrn_reflns_av_unetI/netI     0.0381
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            42446
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        66.292
_diffrn_reflns_theta_max         66.292
_diffrn_reflns_theta_min         3.361
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.147
_exptl_absorpt_correction_T_max  0.720
_exptl_absorpt_correction_T_min  0.498
_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    1.525
_exptl_crystal_description       block
_exptl_crystal_F_000             1631
_exptl_crystal_size_max          0.2567
_exptl_crystal_size_mid          0.1887
_exptl_crystal_size_min          0.1174
_refine_diff_density_max         0.762
_refine_diff_density_min         -0.800
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     837
_refine_ls_number_reflns         12125
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0347
_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^)+(0.0727P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0967
_refine_ls_wR_factor_ref         0.1157
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9962
_reflns_number_total             12125
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02641_si_003.cif
_cod_data_source_block           mf464
_cod_original_cell_volume        3496.17(9)
_cod_database_code               4347037
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         Cu3Br2(P3C32H29)2(CH3CN)2(BF4)(C4H10O)
_reflns_odcompleteness_completeness 97.43
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.81
_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. Uiso/Uaniso restraints and constraints
Uiso(C163) = Uiso(C63)
3. Same fragment restrains
{C63, C64, C65, C66, C67, C68} sigma for 1-2: 0.02, 1-3: 0.04
as
{C163, C164, C165, C166, C167, C168}
{O1, C71, C72} sigma for 1-2: 0.02, 1-3: 0.04
as
{O1, C69, C70}
{O2, C76, C75, C74, C73} sigma for 1-2: 0.02, 1-3: 0.04
as
{O2, C73, C74, C75, C76}
4. Others
 Fixed Sof: C63(0.5) C64(0.5) H64(0.5) C65(0.5) H65(0.5) C66(0.5) H66(0.5)
 C67(0.5) H67(0.5) C68(0.5) H68(0.5) C163(0.5) C164(0.5) H164(0.5) C165(0.5)
 H165(0.5) C166(0.5) H166(0.5) C167(0.5) H167(0.5) C168(0.5) H168(0.5) O1(0.68)
 C69(0.68) H69A(0.68) H69B(0.68) C70(0.68) H70A(0.68) H70B(0.68) H70C(0.68)
 C71(0.68) H71A(0.68) H71B(0.68) C72(0.68) H72A(0.68) H72B(0.68) H72C(0.68)
 O2(0.32) C73(0.32) H73A(0.32) H73B(0.32) C74(0.32) H74A(0.32) H74B(0.32)
 C75(0.32) H75A(0.32) H75B(0.32) C76(0.32) H76A(0.32) H76B(0.32)
5.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C69(H69A,H69B), C71(H71A,
 H71B), C73(H73A,H73B), C74(H74A,H74B), C75(H75A,H75B), C76(H76A,H76B)
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), C164(H164), C165(H165),
 C166(H166), C167(H167), C168(H168)
5.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C70(H70A,H70B,H70C), C72(H72A,H72B,H72C)
;
_olex2_exptl_crystal_mounting_method
'Mounting under cooled galden oil at approx. -60 deg C.'
_olex2_submission_original_sample_id MF464
_olex2_submission_special_instructions 'No special instructions were received'