N,N′-Dimethylene-2,2′-biimidazole—A Mimic of Carboxylate for the Formation of Complexes with Copper(I) And the Anion Directed Formation of a Solvent Pocket
Ferguson, Jayne L.; Fitchett, Christopher M.; Crystal Growth & Design 15 (2015) 1280–; doi:10.1021/cg5016803

data_4512663
_publ_section_title
;
 N,N&#x2032;-Dimethylene-2,2&#x2032;-biimidazole---A Mimic of Carboxylate
 for the Formation of Complexes with Copper(I) And the Anion Directed
 Formation of a Solvent Pocket
;
_journal_issue                   3
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              1280
_journal_paper_doi               10.1021/cg5016803
_journal_volume                  15
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C24 H24 Cu2 N12, 2(B1 F4), 2(C3 H2.5 F0.5)'
_chemical_formula_sum            'C30 H29 B2 Cu2 F9 N12'
_chemical_formula_weight         877.35
_space_group_crystal_system      cubic
_space_group_IT_number           213
_space_group_name_Hall           'P 4bd 2ab 3'
_space_group_name_H-M_alt        'P 41 3 2'
_symmetry_space_group_name_Hall  'P 4bd 2ab 3'
_symmetry_space_group_name_H-M   'P 41 3 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-07-14
_audit_creation_method
;
  Olex2 1.2-beta
  (compiled 2013.04.25 svn.r2679, GUI svn.r4466)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.0849(2)
_cell_length_b                   15.0849(2)
_cell_length_c                   15.0849(2)
_cell_measurement_reflns_used    2214
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      73.6144
_cell_measurement_theta_min      2.9270
_cell_volume                     3432.63(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector_area_resol_mean 21.3001
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -34.00   23.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.9688   38.0000  -30.0000 57

  2 omega   92.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801   45.0000  -60.0000 86

  3 omega -115.00  -65.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.9688  -46.0000 -155.0000 50
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0285706000
_diffrn_orient_matrix_UB_12      0.0753424000
_diffrn_orient_matrix_UB_13      0.0627234000
_diffrn_orient_matrix_UB_21      -0.0980452000
_diffrn_orient_matrix_UB_22      0.0209834000
_diffrn_orient_matrix_UB_23      0.0193193000
_diffrn_orient_matrix_UB_31      0.0014414000
_diffrn_orient_matrix_UB_32      -0.0656020000
_diffrn_orient_matrix_UB_33      0.0782943000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_unetI/netI     0.0194
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3343
_diffrn_reflns_theta_full        66.49
_diffrn_reflns_theta_max         66.49
_diffrn_reflns_theta_min         6.56
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.365
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55868
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.698
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1768
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.545
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.07(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         1019
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0547
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1240P)^2^+1.2113P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1562
_refine_ls_wR_factor_ref         0.1576
_reflns_number_gt                989
_reflns_number_total             1019
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg5016803_si_002.cif
_cod_data_source_block           8
_cod_depositor_comments
'Adding full bibliography for 4512656--4512665.cif.'
_cod_database_code               4512663
_chemical_oxdiff_formula         'C30 H29 N12 F9 B2 Cu'
_reflns_odcompleteness_completeness 100.00
_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. Shared sites
{C1A, C1B}
3. Restrained distances
 F3-C1A
 -1.36 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C1A) = Uanis(C1B)
5. Others
 Fixed Sof: F11(0.16666) F12(0.16666) C1A(0.16667) F1(0.5) F2(0.5) F3(0.16667)
 C1B(0.33333) H1B(0.33333)
6.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B)
6.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7), C1B(H1B)
;