Surfactant-thermal method to prepare two new cobalt metal-organic frameworks
Yu, Xianglin; Toh, Yong Siang; Zhao, Jun; Nie, Lina; Ye, Kaiqi; Wang, Yue; Li, Dongsheng; Zhang, Qichun; Journal of Solid State Chemistry 232 (2015) 14–18; doi:10.1016/j.jssc.2015.08.048

data_1561684
_publ_section_title
;
 Surfactant-thermal method to prepare two new cobalt metal-organic
 frameworks
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              14
_journal_page_last               18
_journal_paper_doi               10.1016/j.jssc.2015.08.048
_journal_volume                  232
_journal_year                    2015
_chemical_formula_sum            'C27 H9 Co3 O18'
_chemical_formula_weight         798.13
_space_group_crystal_system      trigonal
_space_group_IT_number           154
_space_group_name_Hall           'P 32 2"'
_space_group_name_H-M_alt        'P 32 2 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   18.5696(6)
_cell_length_b                   18.5696(6)
_cell_length_c                   12.0128(6)
_cell_measurement_reflns_used    4216
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      21.87
_cell_measurement_theta_min      2.77
_cell_volume                     3587.4(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1003
_diffrn_reflns_av_unetI/netI     0.0770
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            34643
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.914
_diffrn_reflns_theta_min         3.352
_exptl_absorpt_coefficient_mu    1.081
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.108
_exptl_crystal_description       block
_exptl_crystal_F_000             1188
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.359
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details
; 
 Flack x determined using 1548 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.014(14)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         5716
_refine_ls_number_restraints     575
_refine_ls_restrained_S_all      0.950
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0456
_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^)+(0.0579P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1096
_refine_ls_wR_factor_ref         0.1202
_reflns_Friedel_coverage         0.836
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                4041
_reflns_number_total             5716
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            mmc2.cif
_cod_data_source_block           ntu-z33
_cod_original_cell_volume        3587.4(3)
_cod_database_code               1561684
_shelx_estimated_absorpt_t_min   0.659
_shelx_estimated_absorpt_t_max   0.737
_shelxl_version_number           2014/6
_shelx_res_checksum              42426
_shelx_hkl_checksum              66626
_shelx_fab_checksum              42761