A mechanochemically synthesised solid solution enables engineering of the sorption properties of a Werner clathrate
Eustina Batisai; Matteo Lusi; Tia Jacobs; Leonard J. Barbour; Chem.Commun. 48 (2012) 12171–; doi:10.1039/c2cc37261d

data_7108690
_publ_section_title
;
 A mechanochemically synthesised solid solution enables engineering of the
 sorption properties of a Werner clathrate
;
_journal_name_full               Chem.Commun.
_journal_page_first              12171
_journal_paper_doi               10.1039/c2cc37261d
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety         'C44 H36 Cl2 N4 Ni, 0.82(CH3 O)'
_chemical_formula_sum            'C44.82 H38.45 Cl2 N4 Ni O0.82'
_chemical_formula_weight         775.67
_chemical_name_systematic
;
?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.3778(17)
_cell_length_b                   16.212(2)
_cell_length_c                   19.398(3)
_cell_measurement_reflns_used    9086
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      2.32
_cell_volume                     3892.6(9)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'X-Seed (Barbour 2001)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device_type  'Bruker APEX CCD Area Detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_sigmaI/netI    0.0497
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            23493
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         54.928
_diffrn_reflns_theta_min         4.640
_exptl_absorpt_coefficient_mu    0.675
_exptl_absorpt_correction_T_max  0.9294
_exptl_absorpt_correction_T_min  0.928
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2002)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1616.0
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.438
_refine_diff_density_min         -0.531
_refine_diff_density_rms         0.100
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.052(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.174
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         9179
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.174
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0512
_refine_ls_shift/su_max          0.035
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+8.4396P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1071
_refine_ls_wR_factor_ref         0.1158
_reflns_number_gt                8306
_reflns_number_total             9086
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc37261d.txt
_cod_data_source_block           c:2
_cod_original_cell_volume        3892.7(9)
_cod_original_sg_symbol_H-M      P212121
_cod_database_code               7108690