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_4129482
_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
'C92 H76 Co4 N12 O12, 4(N O3), 0.86(C9 H12 O), 1.44(O), 1.57(C9 H11 O)'
_chemical_formula_sum            'C113.82 H103.53 Co4 N16 O27.87'
_chemical_formula_weight         2377.12
_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             2014-03-14
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.12 svn.r2899 for OlexSys, GUI svn.r4794)
;
_cell_angle_alpha                90
_cell_angle_beta                 92.6948(13)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.4463(3)
_cell_length_b                   24.6528(7)
_cell_length_c                   20.3256(6)
_cell_measurement_reflns_used    9844
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.56
_cell_measurement_theta_min      3.59
_cell_volume                     5729.2(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      99.99
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.991
_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  0.0614
_diffrn_reflns_av_unetI/netI     0.0780
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            57396
_diffrn_reflns_point_group_measured_fraction_full 0.904
_diffrn_reflns_point_group_measured_fraction_max 0.927
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         66.604
_diffrn_reflns_theta_min         2.819
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.137
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.4666
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1640 before and 0.0939 after correction.
The Ratio of minimum to maximum transmission is 0.6198.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_F_000             2459
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.990
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.106
_refine_ls_abs_structure_details
;
 Flack x determined using 5934 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.104(3)
_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     1418
_refine_ls_number_reflns         18775
_refine_ls_number_restraints     174
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0579
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0719P)^2^+6.5629P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1452
_refine_ls_wR_factor_ref         0.1529
_reflns_Friedel_coverage         0.823
_reflns_Friedel_fraction_full    0.838
_reflns_Friedel_fraction_max     0.858
_reflns_number_gt                15978
_reflns_number_total             18775
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b06760_si_004.cif
_cod_data_source_block           CMOM_1S_PPex'
_cod_database_code               4129482
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.655
_shelx_estimated_absorpt_t_min   0.385
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O18-H18
 0.87 with sigma of 0.01
 O1-H1
 0.87 with sigma of 0.01
 O2-H2
 0.87 with sigma of 0.01
 O32-H32
 0.87 with sigma of 0.02
 C65-H18
 1.905238 with sigma of 0.02
 O8-H18
 2.02 with sigma of 0.04
 H13A-O10_$1
 2.1 with sigma of 0.04
 C3AB-C32B
 2.53 with sigma of 0.04
 C3AB-C2XB
 2.53 with sigma of 0.04
 C2G-H1
 1.9 with sigma of 0.02
 C10-H2
 1.9 with sigma of 0.02
 H32-C58
 1.9 with sigma of 0.04
 H32-O1N_$1
 2.02 with sigma of 0.04
 C32A-C3AA
 2.53 with sigma of 0.04
 C3AA-C2XA
 2.53 with sigma of 0.04
3. Restrained planarity
 C32B, C2WB, C2XB, C3AB
 with sigma of 0.1
 C2XA, C32A, C2WA, C3AA
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C3FB \\sim C3EB \\sim C3DB: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C3EB \\sim C3EA: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
O14A \\sim C3AA \\sim C33A \\sim C2WA \\sim C39A \\sim C2XA \\sim C32A \\sim
C3BB \\sim C35A \\sim C34B \\sim C35B \\sim O14B \\sim C3AB \\sim C33B \\sim
C2WB \\sim C39B \\sim C2XB \\sim C32B \\sim C3BA \\sim C34A: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C2ZB \\sim O19B \\sim C3DB \\sim H3DB \\sim C3FB \\sim C3EB \\sim H3FA \\sim
H3FB \\sim C2YB \\sim C1HB \\sim H3EA \\sim H3EB \\sim H3EC \\sim H2YB \\sim
C2FB \\sim C3CB \\sim H1HB \\sim H2FB \\sim C30B \\sim H3CB \\sim H30B \\sim
C2ZA \\sim C3DA \\sim H3DA \\sim O19A \\sim C3FA \\sim H3FC \\sim H3FD \\sim
C3EA \\sim C2YA \\sim C1HA \\sim H3ED \\sim H3EE \\sim H3EF \\sim H2YA \\sim
C2FA \\sim H1HA \\sim C3CA \\sim H2FA \\sim C30A \\sim H3CA \\sim H30A: within
1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
5. Others
 Sof(C3DA)=Sof(H3DA)=Sof(O19A)=Sof(C3FA)=Sof(H3FC)=Sof(H3FD)=Sof(C2ZA)=
 Sof(C3EA)=Sof(H3ED)=Sof(H3EE)=Sof(H3EF)=Sof(C2YA)=Sof(H2YA)=Sof(C1HA)=
 Sof(H1HA)=Sof(C2FA)=Sof(H2FA)=Sof(C3CA)=Sof(H3CA)=Sof(C30A)=Sof(H30A)=FVAR(1)
 Sof(O19B)=Sof(C3DB)=Sof(H3DB)=Sof(C3EB)=Sof(H3EA)=Sof(H3EB)=Sof(H3EC)=
 Sof(C3FB)=Sof(H3FA)=Sof(H3FB)=Sof(C2ZB)=Sof(C2YB)=Sof(H2YB)=Sof(C2FB)=
 Sof(H2FB)=Sof(C30B)=Sof(H30B)=Sof(C3CB)=Sof(H3CB)=Sof(C1HB)=Sof(H1HB)=FVAR(2)
 Sof(C22)=Sof(C23)=Sof(H23)=Sof(C25)=Sof(H25)=Sof(C2A)=Sof(H2AA)=Sof(C2B)=
 Sof(H2B)=Sof(C2C)=Sof(H2C)=Sof(C2E)=Sof(H2EA)=Sof(H2EB)=Sof(O13)=Sof(H13A)=
 Sof(C2J)=Sof(H2JA)=Sof(H2JB)=Sof(H2JC)=Sof(C2N)=Sof(H2N)=FVAR(3)
 Sof(O14A)=Sof(C3AA)=Sof(H3AA)=Sof(C33A)=Sof(H33C)=Sof(H33D)=Sof(C39A)=
 Sof(H39D)=Sof(H39E)=Sof(H39F)=Sof(C2WA)=Sof(C2XA)=Sof(H2XA)=Sof(C3BB)=
 Sof(H3BB)=Sof(C34B)=Sof(H34B)=Sof(C35A)=Sof(H35A)=Sof(C32A)=Sof(H32A)=FVAR(4)
 Sof(O14B)=Sof(C33B)=Sof(H33A)=Sof(H33B)=Sof(C2WB)=Sof(C2XB)=Sof(H2XB)=
 Sof(C3BA)=Sof(H3BA)=Sof(C34A)=Sof(H34A)=Sof(C35B)=Sof(H35B)=Sof(C32B)=
 Sof(H32B)=Sof(C39B)=Sof(H39A)=Sof(H39B)=Sof(H39C)=Sof(C3AB)=Sof(H3AB)=Sof(O16)=
 FVAR(5)
6.a Free rotating group:
 O16(O19B,C3DB,C3EB,C3FB,C3DA,O19A,C3FA,C2ZA,C3EA,C2YA,C1HA,C2FA,C3CA,C30A,H32,
 O14A,C3AA,C33A,C39A)
6.b Ternary CH refined with riding coordinates:
 C58(H58), C65(H65), C10(H10), C2G(H2G), C2N(H2N), C3AB(H3AB), C3DB(H3DB),
 C3DA(H3DA), C3AA(H3AA)
6.c Secondary CH2 refined with riding coordinates:
 C2E(H2EA,H2EB), C33B(H33A,H33B), C3FB(H3FA,H3FB), C3FA(H3FC,H3FD), C33A(H33C,
 H33D)
6.d Me refined with riding coordinates:
 C39B(H39A,H39B,H39C), C3EB(H3EA,H3EB,H3EC), C3EA(H3ED,H3EE,H3EF), C39A(H39D,
 H39E,H39F)
6.e Aromatic/amide H refined with riding coordinates:
 C16(H16), C21(H21), C26(H26), C27(H27), C29(H29), C31(H31), C36(H36),
 C37(H37), C38(H38), C43(H43), C47(H47), C49(H49), C50(H50), C51(H51), C53(H53),
  C54(H54), C67(H67), C77(H77), C93(H93), C94(H94), C99(H99), C15(H15), C2(H2A),
  C3(H3), C8(H8), C5(H5), C14(H14), C18(H18A), C11(H11), C13(H13), C17(H17),
 C19(H19), C1A(H1A), C1B(H1B), C1C(H1C), C1E(H1E), C1F(H1F), C1G(H1G), C1I(H1I),
  C1K(H1K), C1P(H1P), C1T(H1T), C1U(H1U), C1V(H1V), C1W(H1W), C1D(H1D),
 C1J(H1J), C1N(H1N), C1O(H1O), C1Q(H1Q), C1R(H1R), C1Y(H1Y), C1Z(H1Z), C23(H23),
  C24(H24), C25(H25), C28(H28), C2A(H2AA), C2B(H2B), C2C(H2C), C2D(H2D),
 C2I(H2I), C2K(H2K), C2L(H2L), C2M(H2M), C2O(H2O), C2P(H2P), C2Q(H2Q), C2R(H2R),
  C2S(H2S), C2T(H2T), C2U(H2U), C2V(H2V), C2XB(H2XB), C3BA(H3BA), C34A(H34A),
 C35B(H35B), C32B(H32B), C2YA(H2YA), C1HA(H1HA), C2FA(H2FA), C3CA(H3CA),
 C30A(H30A), C2YB(H2YB), C2FB(H2FB), C30B(H30B), C3CB(H3CB), C1HB(H1HB),
 C2XA(H2XA), C3BB(H3BB), C34B(H34B), C35A(H35A), C32A(H32A)
6.f Fitted hexagon refined as free rotating group:
 C2WB(C2XB,C3BA,C34A,C35B,C32B), C2ZB(C2YB,C2FB,C30B,C3CB,C1HB), C2WA(C2XA,
 C3BB,C34B,C35A,C32A)
6.g Idealised Me refined as rotating group:
 C2J(H2JA,H2JB,H2JC)
6.h Idealised tetrahedral OH refined as rotating group:
 O13(H13A)
;
_shelx_res_checksum              22378
_shelx_hkl_checksum              33435