Metal organic frameworks from extended, conjugated pentiptycene-based ligands
Crane, Angela K.; White, Nicholas G.; MacLachlan, Mark J.; CrystEngComm 17 (2015) 4912–; doi:10.1039/C5CE00886G

data_7220758
_publ_section_title
;
 Metal organic frameworks from extended, conjugated pentiptycene-based
 ligands
;
_journal_issue                   26
_journal_name_full               CrystEngComm
_journal_page_first              4912
_journal_paper_doi               10.1039/C5CE00886G
_journal_volume                  17
_journal_year                    2015
_chemical_compound_source        synthesized
_chemical_formula_moiety         'C117 H71 N4 O12 Zn2.50'
_chemical_formula_sum            'C117 H71 N4 O12 Zn2.5'
_chemical_formula_weight         1888.32
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_update_record
;
2015-05-06 deposited with the CCDC.
2015-06-02 downloaded from the CCDC.
;
_cell_angle_alpha                88.588(10)
_cell_angle_beta                 73.431(7)
_cell_angle_gamma                66.759(8)
_cell_formula_units_Z            2
_cell_length_a                   17.2471(19)
_cell_length_b                   18.932(3)
_cell_length_c                   21.340(2)
_cell_measurement_reflns_used    4999
_cell_measurement_temperature    90
_cell_measurement_theta_max      50.74
_cell_measurement_theta_min      10.37
_cell_volume                     6106.1(14)
_computing_cell_refinement       'Apex2, (Bruker, 2007)'
_computing_data_collection       'Apex2, (Bruker, 2007)'
_computing_data_reduction        'Apex2, (Bruker, 2007)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      90
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_device       Serial
_diffrn_measurement_device_type  'Bruker Apex Duo'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.080
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12477
_diffrn_reflns_theta_full        44.466
_diffrn_reflns_theta_max         51.110
_diffrn_reflns_theta_min         2.171
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.003
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.662
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2, (Bruker, 2007)'
_exptl_crystal_colour            block
_exptl_crystal_density_diffrn    1.027
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       colourless
_exptl_crystal_F_000             1944
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.12
_refine_diff_density_min         -2.93
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9888
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1222
_refine_ls_number_reflns         11397
_refine_ls_number_restraints     1627
_refine_ls_R_factor_all          0.2095
_refine_ls_R_factor_gt           0.1673
_refine_ls_shift/su_max          0.0004278
_refine_ls_shift/su_mean         0.0000115
_refine_ls_structure_factor_coef Fsqd
_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: 
 600. 890. 418. 101. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3903
_refine_ls_wR_factor_gt          0.3658
_refine_ls_wR_factor_ref         0.3903
_reflns_limit_h_max              17
_reflns_limit_h_min              -16
_reflns_limit_k_max              19
_reflns_limit_k_min              -19
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                7346
_reflns_number_total             8955
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   4.33
_oxford_diffrn_Wilson_scale      2.45
_oxford_refine_ls_r_factor_ref   0.2095
_oxford_refine_ls_scale          1.079(9)
_oxford_reflns_number_all        11397
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            c5ce00886g2.cif
_cod_data_source_block           PMOF3
_cod_depositor_comments
'Adding full bibliography for 7220756--7220758.cif.'
_cod_original_cell_volume        6105.9(14)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C117 H71 N4 O12 Zn2.50'
_cod_database_code               7220758