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_4347041
_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         'C78 H68 Cu3 I2 Mo2 O4 P12, B F4'
_chemical_formula_sum            'C78 H68 B Cu3 F4 I2 Mo2 O4 P12'
_chemical_formula_weight         2164.07
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-01-11
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90.0
_cell_angle_beta                 99.9325(9)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   23.7257(2)
_cell_length_b                   15.12645(14)
_cell_length_c                   26.4442(2)
_cell_measurement_reflns_used    38532
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      73.5060
_cell_measurement_theta_min      3.3780
_cell_volume                     9348.20(14)
_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)'
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_diffrn_ambient_temperature      123(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3546
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_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_details
;
  1 omega -119.00  -12.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8939  -77.0000 -120.0000 214

  2 omega  -88.00  -44.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8939  113.0000   89.0000 88

  3 omega  -63.00   27.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8939   37.0000 -180.0000 180

  4 omega   79.00  115.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   45.0000  -30.0000 72

  5 omega   45.00   72.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -45.0000   30.0000 54

  6 omega   60.00  108.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800 -113.0000   -1.0000 96

  7 omega   42.00   77.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -45.0000    0.0000 70

  8 omega   32.00   77.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -45.0000  -60.0000 90

  9 omega   79.00  156.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   45.0000  -60.0000 154

 10 omega  132.00  158.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   45.0000  -30.0000 52

 11 omega   50.00  156.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   15.0000 -120.0000 212

 12 omega  109.00  158.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  125.0000  150.0000 98

 13 omega -117.00  -15.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8939  -37.0000  -60.0000 204

 14 omega  -67.00   35.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8939   37.0000    0.0000 204

 15 omega -120.00   -7.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8939  -77.0000   90.0000 226

 16 omega   73.00  158.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   77.0000   30.0000 170

 17 omega   73.00  158.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   77.0000   90.0000 170

 18 omega   32.00   77.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -45.0000   90.0000 90

 19 omega   32.00   57.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -45.0000 -150.0000 50

 20 omega   32.00   77.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -45.0000  150.0000 90
;
_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      0.0317865000
_diffrn_orient_matrix_UB_12      -0.0352232000
_diffrn_orient_matrix_UB_13      -0.0419685000
_diffrn_orient_matrix_UB_21      0.0545774000
_diffrn_orient_matrix_UB_22      -0.0122669000
_diffrn_orient_matrix_UB_23      0.0403565000
_diffrn_orient_matrix_UB_31      -0.0188523000
_diffrn_orient_matrix_UB_32      -0.0947811000
_diffrn_orient_matrix_UB_33      0.0103964000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0437
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            18479
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.719
_diffrn_reflns_theta_min         3.379
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.435
_exptl_absorpt_correction_T_max  0.648
_exptl_absorpt_correction_T_min  0.204
_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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_description
;
;
_exptl_crystal_F_000             4264
_exptl_crystal_size_max          0.2669
_exptl_crystal_size_mid          0.0738
_exptl_crystal_size_min          0.0468
_refine_diff_density_max         2.353
_refine_diff_density_min         -1.157
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     949
_refine_ls_number_reflns         18479
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0523
_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^)+(0.0954P)^2^+26.7988P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1441
_refine_ls_wR_factor_ref         0.1527
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16136
_reflns_number_total             18479
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02641_si_012.cif
_cod_data_source_block           mf119_new_sq_s
_cod_database_code               4347041
_chemical_oxdiff_formula         Cu3I2(P3C32H29)2(BF4)(MoP3C7O2H5)2(CH2Cl2)2.5
_reflns_odcompleteness_completeness 99.89
_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
 F6-B2 = F5-B2 = F8-B2 = F7-B2 = F2-B1 = F3-B1 = F1-B1 = F4-B1
 1.33 with sigma of 0.02
 F1-F2 = F1-F3 = F1-F4 = F2-F3 = F2-F4 = F3-F4
 2.26 with sigma of 0.04
 F5-F6 = F5-F7 = F5-F8 = F6-F7 = F6-F8 = F7-F8
 2.26 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C7) \\sim Ueq, Uanis(O2) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uiso(F2) = Uiso(F8)
4. Others
 Fixed Sof: F1(0.5) F3(0.5) F2(0.5) F4(0.5) B1(0.5) F5(0.5) F7(0.5) F8(0.5)
 F6(0.5) B2(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C17(H17a,H17b), C18(H18a,H18b), C16(H16a,H16b), C15(H15a,H15b)
5.b Aromatic/amide H refined with riding coordinates:
 C30(H30), C21(H21), C39(H39), C38(H38), C42(H42), C20(H20), C32(H32),
 C64(H64), C33(H33), C68(H68), C48(H48), C70(H70), C62(H62), C72(H72), C45(H45),
  C36(H36), C63(H63), C66(H66), C71(H71), C65(H65), C47(H47), C52(H52),
 C26(H26), C69(H69), C23(H23), C29(H29), C44(H44), C34(H34), C12(H12), C40(H40),
  C78(H78), C24(H24), C54(H54), C46(H46), C74(H74), C59(H59), C75(H75),
 C56(H56), C60(H60), C9(H9), C77(H77), C22(H22), C27(H27), C2(H2), C5(H5),
 C1(H1), C76(H76), C41(H41), C10(H10), C35(H35), C51(H51), C4(H4), C28(H28),
 C3(H3), C57(H57), C8(H8), C58(H58), C11(H11), C53(H53), C50(H50)
;
_shelx_fab_checksum              1487
_shelx_shelxl_version_number     2014/7
_olex2_submission_original_sample_id MF119
_olex2_submission_special_instructions 'No special instructions were received'