Structural Insight into Guest Binding Sites in a Porous Homochiral Metal-Organic Material.
Zhang, Shi-Yuan; Wojtas, Lukasz; Zaworotko, Michael J.; Journal of the American Chemical Society 137 (2015) 12045–12049; doi:10.1021/jacs.5b06760

data_4129481
_publ_section_title
;
 Structural Insight into Guest Binding Sites in a Porous Homochiral
 Metal-Organic Material.
;
_journal_issue                   37
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12045
_journal_page_last               12049
_journal_paper_doi               10.1021/jacs.5b06760
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety
'C46 H38 Co2 N6 O6, 2(N O3), 2.41(C6 H5 N O2)'
_chemical_formula_sum            'C60.4 H50 Co2 N10.4 O16.8'
_chemical_formula_weight         1308.18
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2014-03-19
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.12 svn.r2899 for OlexSys, GUI svn.r4796)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.106(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.2416(6)
_cell_length_b                   24.9560(15)
_cell_length_c                   11.4453(7)
_cell_measurement_reflns_used    9861
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.62
_cell_measurement_theta_min      3.54
_cell_volume                     2924.8(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.01
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_av_unetI/netI     0.0566
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            27521
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        65.975
_diffrn_reflns_theta_max         66.637
_diffrn_reflns_theta_min         3.542
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.140
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.4116
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1365 before and 0.0910 after correction.
The Ratio of minimum to maximum transmission is 0.5468.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_F_000             1347
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.906
_refine_diff_density_min         -0.891
_refine_diff_density_rms         0.124
_refine_ls_abs_structure_details
;
 Flack x determined using 3541 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.184(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     763
_refine_ls_number_reflns         9068
_refine_ls_number_restraints     178
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0862
_refine_ls_R_factor_gt           0.0840
_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^)+(0.0258P)^2^+30.5743P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2000
_refine_ls_wR_factor_ref         0.2012
_reflns_Friedel_coverage         0.917
_reflns_Friedel_fraction_full    0.964
_reflns_Friedel_fraction_max     0.964
_reflns_number_gt                8763
_reflns_number_total             9068
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b06760_si_003.cif
_cod_data_source_block           CMOM_1R_NB
_cod_original_formula_sum        'C60.40 H50 Co2 N10.40 O16.80'
_cod_database_code               4129481
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.821
_shelx_estimated_absorpt_t_min   0.577
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 O14-H14
 0.88 with sigma of 0.01
 O16-H16
 0.88 with sigma of 0.02
 O18-N10
 1.22 with sigma of 0.02
 N5B-C1N
 1.47 with sigma of 0.02
 O21-N21 = O19-N21
 1.22 with sigma of 0.02
 C1V-C1Y
 1.39 with sigma of 0.02
 C1X-N21
 1.47 with sigma of 0.02
 H47-H16
 -2.2 with sigma of 0.02
 C25-H14
 1.916801 with sigma of 0.02
 Co2-H14
 2.896002 with sigma of 0.02
3. Rigid bond restraints
 N3, C10, C24
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
O12 \\sim N5B: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04
C37 \\sim C54 \\sim C31 \\sim N15 \\sim C28 \\sim C60: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
O1 \\sim C23 \\sim O5 \\sim C47: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C3 \\sim C1B \\sim C15 \\sim C4 \\sim C6 \\sim C5: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08
C17 \\sim C22 \\sim C13: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Uiso(O18) = Uiso(N5B)
5. Rigid body (RIGU) restrains
 O11, N2, O15, C1F, C1E, C1H, C1D, C1G, C1C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C1U)=Sof(C1W)=Sof(H1W)=Sof(C1L)=Sof(H1L)=Sof(C1K)=Sof(H1K)=Sof(C1T)=
 Sof(H1T)=Sof(C1R)=Sof(H1R)=Sof(N10)=Sof(O17)=Sof(O18)=FVAR(1)
 Sof(C1N)=Sof(C1P)=Sof(H1P)=Sof(C1M)=Sof(H1M)=Sof(C1J)=Sof(H1J)=Sof(C1I)=
 Sof(H1I)=Sof(C1O)=Sof(H1O)=Sof(O12)=Sof(N5B)=Sof(O13)=FVAR(2)
 Sof(C1X)=Sof(C1S)=Sof(H1S)=Sof(C1Q)=Sof(H1Q)=Sof(C62)=Sof(H62)=Sof(C1Y)=
 Sof(H1Y)=Sof(C1V)=Sof(H1V)=Sof(N21)=Sof(O19)=Sof(O21)=FVAR(3)
7.a Ternary CH refined with riding coordinates:
 C25(H25), C47(H47)
7.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C12(H12), C13(H13), C20(H20), C22(H22), C24(H24), C26(H26),
 C27(H27), C28(H28), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35),
  C42(H42), C46(H46), C54(H54), C58(H58), C60(H60), C61(H61), C1(H1), C4(H4),
 C5(H5), C3(H3), C14(H14A), C18(H18), C7(H7), C11(H11), C15(H15), C16(H16A),
 C1A(H1A), C1B(H1B), C1E(H1E), C1H(H1H), C1D(H1D), C1G(H1G), C1C(H1C), C1P(H1P),
  C1M(H1M), C1J(H1J), C1I(H1I), C1O(H1O), C1W(H1W), C1L(H1L), C1K(H1K),
 C1T(H1T), C1R(H1R), C1S(H1S), C1Q(H1Q), C62(H62), C1Y(H1Y), C1V(H1V)
7.c Fitted hexagon refined as free rotating group:
 C1F(C1E,C1H,C1D,C1G,C1C), C1N(C1P,C1M,C1J,C1I,C1O), C1U(C1W,C1L,C1K,C1T,C1R),
 C1X(C1S,C1Q,C62,C1Y,C1V)
;
_shelx_res_checksum              25309
_shelx_hkl_checksum              37867