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_4347040
_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
'B F4, C84 H88 Cu3 Fe2 I2 P16, 2.29(C H2 Cl2)'
_chemical_formula_sum            'C86.29 H92.58 B Cl4.58 Cu3 F4 Fe2 I2 P16'
_chemical_formula_weight         2430.47
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2015-07-16
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 98.126(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.5036(5)
_cell_length_b                   15.3314(3)
_cell_length_c                   26.5971(6)
_cell_measurement_reflns_used    28180
_cell_measurement_temperature    123.0(2)
_cell_measurement_theta_max      66.7360
_cell_measurement_theta_min      3.3430
_cell_volume                     9891.5(4)
_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      123.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3546
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_details
;
  1 omega  -88.00   -7.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.0814  125.0000  -60.0000 162

  2 omega  -28.00   56.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       41.0814  -37.0000 -150.0000 168

  3 omega   62.00  135.00   0.5000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       92.6403   61.0000   90.0000 146

  4 omega   18.00   77.00   0.5000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       92.6403  -45.0000 -180.0000 118

  5 omega   28.00   71.00   0.5000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       92.6403  -45.0000   90.0000 86

  6 omega   70.00  150.00   0.5000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       92.6403   45.0000   30.0000 160

  7 omega   87.00  158.00   0.5000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       92.6403  125.0000  -60.0000 142

  8 omega   21.00   72.00   0.5000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       92.6403  -45.0000  -90.0000 102

  9 omega -120.00   -7.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.0814  -77.0000  -60.0000 226

 10 omega -117.00  -15.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.0814  -37.0000  150.0000 204

 11 omega   18.00   77.00   0.5000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       92.6403  -45.0000    0.0000 118

 12 omega   62.00  117.00   0.5000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       92.6403   61.0000  150.0000 110

 13 omega   65.00  158.00   0.5000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       92.6403   45.0000  -90.0000 186
;
_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      0.0179640000
_diffrn_orient_matrix_UB_12      -0.0524548000
_diffrn_orient_matrix_UB_13      0.0490163000
_diffrn_orient_matrix_UB_21      0.0583244000
_diffrn_orient_matrix_UB_22      -0.0093396000
_diffrn_orient_matrix_UB_23      -0.0146124000
_diffrn_orient_matrix_UB_31      0.0174219000
_diffrn_orient_matrix_UB_32      0.0851626000
_diffrn_orient_matrix_UB_33      0.0285255000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0671
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_Laue_measured_fraction_full 0.961
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            51872
_diffrn_reflns_point_group_measured_fraction_full 0.961
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        66.850
_diffrn_reflns_theta_max         66.850
_diffrn_reflns_theta_min         3.336
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.902
_exptl_absorpt_correction_T_max  0.700
_exptl_absorpt_correction_T_min  0.322
_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 green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_description       prism
_exptl_crystal_F_000             4857
_exptl_crystal_size_max          0.188
_exptl_crystal_size_mid          0.0679
_exptl_crystal_size_min          0.034
_refine_diff_density_max         2.511
_refine_diff_density_min         -1.956
_refine_diff_density_rms         0.237
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1132
_refine_ls_number_reflns         16887
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.1111
_refine_ls_R_factor_gt           0.1027
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0069P)^2^+544.3885P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2593
_refine_ls_wR_factor_ref         0.2633
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14515
_reflns_number_total             16887
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02641_si_014.cif
_cod_data_source_block           mf225_new_dr2
_cod_database_code               4347040
_chemical_oxdiff_formula         Cu3I2(P3C32H29)2(C10H15FeP5)2(BF4)(CH2Cl2)2
_reflns_odcompleteness_completeness 95.38
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl7-C88 = Cl6-C88
 1.72 with sigma of 0.02
 Cl7-Cl6
 2.92 with sigma of 0.02
 Cl5-Cl8
 2.92 with sigma of 0.02
 Cl3-Cl4
 2.92 with sigma of 0.02
 Cl3-C99 = Cl4-C99 = Cl8-C87 = Cl5-C87
 1.72 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C99) \\sim Ueq, Uanis(C87) \\sim Ueq, Uanis(Cl3) \\sim Ueq: with sigma of
0.05 and sigma for terminal atoms of 0.1
Uanis(Cl4) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(B1) \\sim Ueq, Uanis(F1) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(Cl8) = Uanis(Cl5)
Uiso(F6) = Uiso(F7) = Uiso(F5) = Uiso(F8) = Uiso(B2)
4. Same fragment restrains
{F1, F2, F3, F4, B1} sigma for 1-2: 0.02, 1-3: 0.04
as
{F5, F6, F7, F8, B2}
5. Others
 Fixed Sof: F1(0.65) F2(0.65) F3(0.65) F4(0.65) B1(0.65) F5(0.35) F6(0.35)
 F7(0.35) F8(0.35) B2(0.35) Cl5(0.58) Cl3(0.42) Cl6(0.29) C99(0.42) H99A(0.42)
 H99B(0.42) C87(0.58) H87A(0.58) H87B(0.58) C88(0.29) H88A(0.29) H88B(0.29)
 Cl4(0.42) Cl8(0.58) Cl7(0.29)
6.a Secondary CH2 refined with riding coordinates:
 C99(H99A,H99B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,
 H24B), C85(H85A,H85B), C87(H87A,H87B), C88(H88A,H88B)
6.b Aromatic/amide H refined with riding coordinates:
 C70(H70), C81(H81), C45(H45), C39(H39), C64(H64), C53(H53), C80(H80),
 C33(H33), C76(H76), C28(H28), C48(H48), C56(H56), C72(H72), C44(H44), C52(H52),
  C60(H60), C68(H68), C42(H42), C46(H46), C50(H50), C54(H54), C58(H58),
 C62(H62), C66(H66), C74(H74), C78(H78), C47(H47), C51(H51), C26(H26), C27(H27),
  C57(H57), C82(H82), C59(H59), C83(H83), C63(H63), C65(H65), C69(H69),
 C71(H71), C35(H35), C36(H36), C75(H75), C77(H77), C38(H38), C40(H40), C41(H41),
  C84(H84), C29(H29), C30(H30), C32(H32), C34(H34)
6.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,
 H10B,H10C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C)
;
_shelx_shelxl_version_number     2014/7
_olex2_exptl_crystal_mounting_method 'mineral oil'
_olex2_submission_original_sample_id MF225
_olex2_submission_special_instructions 'No special instructions were received'