Resin-assisted solvothermal synthesis of transition metal-organic frameworks.
Du, Yi; Thompson, Amber L.; Russell, Nicola; O'Hare, Dermot; Dalton transactions (Cambridge, England : 2003) 39 (2010) 3384–3395; doi:10.1039/b919675g

data_7024644
_publ_section_title
;
 Resin-assisted solvothermal synthesis of transition metal-organic
 frameworks.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3384
_journal_page_last               3395
_journal_paper_doi               10.1039/b919675g
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C56 H32 Co3 O16'
_chemical_formula_sum            'C56 H32 Co3 O16'
_chemical_formula_weight         1137.66
_chemical_melting_point          ?
_space_group_IT_number           52
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2a 2bc'
_symmetry_space_group_name_H-M   'P n n a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             08-09-30
_audit_creation_method           CRYSTALS_ver_12.86
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.09860(10)
_cell_length_b                   22.3068(3)
_cell_length_c                   13.8496(3)
_cell_measurement_reflns_used    9966
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     8062.9(2)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.091
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            143130
_diffrn_reflns_theta_full        26.978
_diffrn_reflns_theta_max         27.528
_diffrn_reflns_theta_min         5.198
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.656
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.74
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            clear_intense_purple
_exptl_crystal_density_diffrn    0.937
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2308
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;
The discrete Fourier transform of the void region were treated as
contributions to the A and B parts of the calculated structure factors.
;
_refine_diff_density_max         0.83
_refine_diff_density_min         -0.65
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0007
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         7670
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0808
_refine_ls_R_factor_gt           0.0732
_refine_ls_shift/su_max          0.000721
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
1.39 1.05 0.824
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0852
_refine_ls_wR_factor_gt          0.0765
_refine_ls_wR_factor_ref         0.0753
_reflns_limit_h_max              33
_reflns_limit_h_min              0
_reflns_limit_k_max              0
_reflns_limit_k_min              -28
_reflns_limit_l_max              17
_reflns_limit_l_min              -17
_reflns_number_gt                8078
_reflns_number_total             9176
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.67
_oxford_diffrn_Wilson_scale      24.83
_oxford_refine_ls_r_factor_ref   0.0707
_oxford_refine_ls_scale          0.2428(5)
_oxford_reflns_number_all        9272
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_oxford_structure_analysis_title 5731
_cod_data_source_file            b919675g.txt
_cod_data_source_block           6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_symmetry_cell_setting' value
'Orthorhombic' changed to 'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P n n a '
_cod_database_code               7024644