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_4347036
_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 Cl2 Cu3 P6, C H2 Cl2, B F4'
_chemical_formula_sum            'C65 H60 B Cl4 Cu3 F4 P6'
_chemical_formula_weight         1446.18
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-07-14
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 114.0862(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.60512(13)
_cell_length_b                   31.7652(2)
_cell_length_c                   14.05170(13)
_cell_measurement_reflns_used    92906
_cell_measurement_temperature    123.02(10)
_cell_measurement_theta_max      76.4010
_cell_measurement_theta_min      3.5240
_cell_volume                     6358.96(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_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      123.02(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1773
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
  1 omega -115.00  -16.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
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  2 omega  -54.00   33.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
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  3 omega  -31.00   70.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
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  4 omega    2.00   97.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       41.4171 -125.0000 -120.0000 190

  5 omega   29.00  109.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000 -180.0000 160

  6 omega   84.00  109.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
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  7 omega   40.00   77.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
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  8 omega  115.00  147.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
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  9 omega   48.00   77.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
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 10 omega   36.00  143.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -77.0000  -60.0000 214

 11 omega   36.00  112.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000    0.0000 -150.0000 152

 12 omega   62.00  116.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000   90.0000 108

 13 omega   36.00  114.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
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 14 omega  116.00  158.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
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 15 omega   29.00  109.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000  120.0000 160

 16 omega   84.00  153.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
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 17 omega   86.00  158.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
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 18 omega  100.00  126.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
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 19 omega   46.00  141.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -61.0000  150.0000 190

 20 omega   65.00  143.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
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 21 omega   40.00   89.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
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 22 omega -115.00  -13.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.4171  -57.0000 -180.0000 204

 23 omega -115.00  -13.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.4171  -57.0000   90.0000 204

 24 omega  -97.00   -2.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.4171  125.0000  -30.0000 190

 25 omega -115.00  -13.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.4171  -57.0000  -90.0000 204

 26 omega   36.00   69.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000    0.0000 66

 27 omega   36.00   69.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000  -30.0000 66

 28 omega   36.00   69.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000 -180.0000 66

 29 omega   83.00  158.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   61.0000  150.0000 150

 30 omega   86.00  158.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   45.0000  -90.0000 144

 31 omega   39.00   77.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000   60.0000 76

 32 omega   83.00  158.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   61.0000   90.0000 150

 33 omega   36.00   69.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000  150.0000 66

 34 omega   36.00   69.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000  -90.0000 66

 35 omega   83.00  158.00   0.5000    8.0000
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    -      112.0000   61.0000  -60.0000 150

 36 omega   86.00  158.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   45.0000   30.0000 144

 37 omega   79.00  158.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000  -30.0000 158

 38 omega -118.00   -9.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.4171  -77.0000 -120.0000 218

 39 omega -118.00   -9.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.4171  -77.0000  150.0000 218

 40 omega    9.00  118.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       41.4171   77.0000  120.0000 218

 41 omega    2.00   97.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       41.4171 -125.0000 -120.0000 190

 42 omega   79.00  158.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000  -90.0000 158

 43 omega   83.00  158.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   61.0000   60.0000 150

 44 omega   83.00  158.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   61.0000  120.0000 150

 45 omega   36.00  116.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000  120.0000 160

 46 omega   83.00  158.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   61.0000 -180.0000 150

 47 omega   39.00   77.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000  -60.0000 76

 48 omega   29.00  109.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000  -60.0000 160

 49 omega   39.00   77.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000 -180.0000 76

 50 omega   83.00  158.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   61.0000  -30.0000 150

 51 omega   83.00  158.00   0.5000    8.0000
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 52 omega   83.00  158.00   0.5000    8.0000
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 53 omega   86.00  158.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   45.0000 -120.0000 144

 54 omega -116.00  -17.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.4171  -37.0000  -60.0000 198

 55 omega -118.00   -9.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.4171  -77.0000   90.0000 218

 56 omega  -33.00   66.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       41.4171  -37.0000 -120.0000 198

 57 omega   10.00  116.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       41.4171   72.0000   41.9263 212

 58 omega   83.00  158.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
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 59 omega   79.00  109.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
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 60 omega   29.00  109.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000 -150.0000 160
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0671865000
_diffrn_orient_matrix_UB_12      0.0241681000
_diffrn_orient_matrix_UB_13      0.0967345000
_diffrn_orient_matrix_UB_21      0.0685429000
_diffrn_orient_matrix_UB_22      0.0064731000
_diffrn_orient_matrix_UB_23      -0.0524567000
_diffrn_orient_matrix_UB_31      -0.0498240000
_diffrn_orient_matrix_UB_32      0.0415420000
_diffrn_orient_matrix_UB_33      -0.0481069000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0659
_diffrn_reflns_av_unetI/netI     0.0204
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            133342
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.067
_diffrn_reflns_theta_max         67.067
_diffrn_reflns_theta_min         3.400
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.565
_exptl_absorpt_correction_T_max  0.614
_exptl_absorpt_correction_T_min  0.356
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
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    1.511
_exptl_crystal_description       block
_exptl_crystal_F_000             2944
_exptl_crystal_size_max          0.3674
_exptl_crystal_size_mid          0.1951
_exptl_crystal_size_min          0.1611
_refine_diff_density_max         0.836
_refine_diff_density_min         -0.562
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     824
_refine_ls_number_reflns         11350
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0324
_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^)+(0.0509P)^2^+6.4755P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0888
_refine_ls_wR_factor_ref         0.0899
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10660
_reflns_number_total             11350
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02641_si_002.cif
_cod_data_source_block           ld039_new
_cod_original_cell_volume        6358.95(11)
_cod_database_code               4347036
_chemical_oxdiff_formula         Cu3Cl2(P3C32H29)2BF4(CH2Cl2)
_reflns_odcompleteness_completeness 99.97
_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
 Cl5-C901 = Cl6-C901 = Cl3-C900 = Cl4-C900
 1.72 with sigma of 0.02
3. Others
 Fixed Sof: C42(0.5) H42(0.5) C43(0.5) H43(0.5) C44(0.5) H44(0.5) C142(0.5)
 H142(0.5) C143(0.5) H143(0.5) C144(0.5) H144(0.5) Cl3(0.62) Cl4(0.62)
 C900(0.62) H90A(0.62) H90B(0.62) Cl5(0.38) Cl6(0.38) C901(0.38) H90C(0.38)
 H90D(0.38) F2(0.6) F3(0.6) F4(0.6) F5(0.4) F6(0.4) F7(0.4)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C900(H90A,H90B),
 C901(H90C,H90D)
4.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), 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), C42(H42), C43(H43), C44(H44), C142(H142), C143(H143), C144(H144)
;
_shelx_shelxl_version_number     2014/7
_olex2_exptl_crystal_mounting_method 'mineral oil'
_olex2_submission_original_sample_id LD039
_olex2_submission_special_instructions 'No special instructions were received'