Coordination polymers constructed from tetrahedral-shaped adamantane tectons
Mocanu, Teodora; Pop, Lidia; Hădade, Niculina D.; Shova, Sergiu; Grosu, Ion; Andruh, Marius; CrystEngComm 19 (2017) 27–; doi:10.1039/C6CE02146H

data_7227200
_publ_section_title
;
 Coordination polymers constructed from tetrahedral-shaped adamantane
 tectons
;
_journal_issue                   1
_journal_name_full               CrystEngComm
_journal_page_first              27
_journal_paper_doi               10.1039/C6CE02146H
_journal_volume                  19
_journal_year                    2017
_chemical_formula_moiety
'0.5(C108 H96 Cu2 N8 O4), 2(B0.5 F2), B0.5 F1.93, 0.5(F), 0.5(B F3), 2(H2 O)'
_chemical_formula_sum            'C54 H52 B2 Cu F7.97 N4 O4'
_chemical_formula_weight         1057.54
_space_group_crystal_system      tetragonal
_space_group_IT_number           97
_space_group_name_Hall           'I 4 2'
_space_group_name_H-M_alt        'I 4 2 2'
_symmetry_space_group_name_Hall  'I 4 2'
_symmetry_space_group_name_H-M   'I 4 2 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-09-19
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2016-11-18 deposited with the CCDC.
2016-11-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8199(9)
_cell_length_b                   12.8199(9)
_cell_length_c                   32.617(4)
_cell_measurement_reflns_used    1423
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      67.1770
_cell_measurement_theta_min      4.8730
_cell_volume                     5360.6(8)
_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, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0851
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega  -72.00  -43.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  158.0000  -81.0000 29

  2 omega   26.00   66.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -120.0000 40

  3 omega  -12.00   40.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  120.0000 52

  4 omega   -7.00   67.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000  -30.0000 74

  5 omega   20.00  114.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   19.0000  -90.0000 94

  6 omega   93.00  120.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000   60.0000 27

  7 omega    4.00   95.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -99.0000  -90.0000 91

  8 omega   90.00  175.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   50.0000    0.0000 85

  9 omega   36.00   63.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -28.0000  110.0000 27

 10 omega   83.00  159.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   25.0000  -30.0000 76

 11 omega   54.00   89.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -37.0000  120.0000 35

 12 omega   87.00  162.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000  -90.0000 75
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1111608000
_diffrn_orient_matrix_UB_12      0.0422638000
_diffrn_orient_matrix_UB_13      -0.0069222000
_diffrn_orient_matrix_UB_21      -0.0219478000
_diffrn_orient_matrix_UB_22      0.0088534000
_diffrn_orient_matrix_UB_23      -0.0462936000
_diffrn_orient_matrix_UB_31      -0.0401612000
_diffrn_orient_matrix_UB_32      0.1120932000
_diffrn_orient_matrix_UB_33      0.0062372000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_av_unetI/netI     0.0596
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            6049
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        58.904
_diffrn_reflns_theta_max         58.904
_diffrn_reflns_theta_min         3.705
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.218
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.35289
_exptl_absorpt_correction_type   multi-scan
_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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_description       plate
_exptl_crystal_F_000             2187
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.258
_refine_diff_density_min         -0.244
_refine_diff_density_rms         0.103
_refine_ls_abs_structure_details
;
 Flack x determined using 313 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.42(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     169
_refine_ls_number_reflns         1932
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      3.153
_refine_ls_R_factor_all          0.1507
_refine_ls_R_factor_gt           0.1033
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2671
_refine_ls_wR_factor_ref         0.3199
_reflns_Friedel_coverage         0.664
_reflns_Friedel_fraction_full    0.991
_reflns_Friedel_fraction_max     0.991
_reflns_number_gt                1169
_reflns_number_total             1932
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce02146h2.cif
_cod_data_source_block           shc_475_maan_1
_cod_depositor_comments
'Adding full bibliography for 7227200--7227201.cif.'
_cod_original_cell_volume        5360.5(10)
_cod_database_code               7227200
_chemical_oxdiff_formula         'C25 H20 N4 B1 F4 O6 Cu1'
_chemical_oxdiff_usercomment     TM_6
_reflns_odcompleteness_completeness 99.30
_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 O(H,H) groups
2. Restrained distances
 B2-B2
 1.2 with sigma of 0.01
 B6-B5
 1 with sigma of 0.01
 F1-F2
 2.2 with sigma of 0.01
 F2-B1 = F1-B1
 1.4 with sigma of 0.01
 F6-B3 \\sim B4-F6
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uiso(F1) = Uiso(B1)
Uiso(F4) = Uiso(F3) = Uiso(B2) = Uiso(B4) = Uiso(F6) = Uiso(F5) = Uiso(B5) =
Uiso(F8) = Uiso(F7) = Uiso(B6) = Uiso(F9) = Uiso(B3)
4. Others
 Fixed Sof: H2A(0.5) H2B(0.5) H4A(0.5) H4B(0.5) H8A(0.5) H8B(0.5) H1WA(0.5)
 H1WB(0.5) B5(0.0625) B4(0.0625) F7(0.125) F3(0.28125) B3(0.0625) O12(0.5)
 H12A(0.5) H12B(0.5) F1(0.125) B1(0.125) F2(0.375) F8(0.375) F6(0.375)
 B6(0.0625) B2(0.125) F4(0.094) F9(0.125)
 Fixed Z: F7(0.28486)
5.a Riding coordinates:
 O1W(H1WA,H1WB), O12(H12A,H12B)
5.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C4(H4A,H4B), C8(H8A,H8B)
5.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C18(H18)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-03-03
_olex2_submission_special_instructions 'No special instructions were received'