Stereochemistry of cage amine complexes ‒ probing the ligand conformational flexibility with hydrogen bonds
Ling, Irene; Sobolev, Alexandre N.; Hashim, Rauzah; Harrowfield, Jack M.; CrystEngComm 16 (2014) 11058–; doi:10.1039/C4CE01980F

data_7218681
_publ_section_title
;
 Stereochemistry of cage amine complexes -- probing the ligand
 conformational flexibility with hydrogen bonds
;
_journal_issue                   48
_journal_name_full               CrystEngComm
_journal_page_first              11058
_journal_paper_doi               10.1039/C4CE01980F
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety         '2(C14 H30 Cl2 Co N6), 5Cl, Br, 5(H2 O)'
_chemical_formula_sum            'C28 H70 Br Cl9 Co2 N12 O5'
_chemical_formula_weight         1171.78
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
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_symmetry_space_group_name_Hall  '-P 2ybc'
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_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.0
_cell_angle_beta                 117.183(5)
_cell_angle_gamma                90.0
_cell_formula_units_Z            2
_cell_length_a                   9.7649(4)
_cell_length_b                   27.6067(8)
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_cell_measurement_reflns_used    14130
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.73
_cell_measurement_theta_min      3.76
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_computing_cell_refinement
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
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_computing_data_collection
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_reduction
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_molecular_graphics    'Mercury CSD v. 2.3 (2009)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.0009
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur-S, Sapphire CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_av_sigmaI/netI    0.0638
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            40659
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         30.75
_diffrn_reflns_theta_min         3.80
_exptl_absorpt_coefficient_mu    2.170
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79889
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.697
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.158
_refine_diff_density_min         -1.491
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         6677
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0873
_refine_ls_R_factor_gt           0.0543
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1532
_refine_ls_wR_factor_ref         0.1622
_reflns_number_gt                4501
_reflns_number_total             6677
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ce01980f1.cif
_cod_data_source_block           cmpnd02
_cod_depositor_comments
'Adding full bibliography for 7218680--7218682.cif.'
_cod_original_cell_volume        2293.59(15)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7218681