Network diversity through two-step crystal engineering of a decorated 6-connected primary molecular building block
Yang, Qing-Yuan; Chen, Kai-Jie; Schoedel, Alexander; Wojtas, Lukasz; Perry IV, John J.; Zaworotko, Michael J.; CrystEngComm 18 (2016) 8578–; doi:10.1039/C6CE01544A

data_7236182
_publ_section_title
;
 Network diversity through two-step crystal engineering of a decorated
 6-connected primary molecular building block
;
_journal_issue                   44
_journal_name_full               CrystEngComm
_journal_page_first              8578
_journal_paper_doi               10.1039/C6CE01544A
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety
'0.17(C612 H708 Cl84 Cr36 Cu36 N132 O216), 5(C3 H7 N O), 1(O)'
_chemical_formula_sum            'C117 H155 Cl14 Cr6 Cu6 N27 O42'
_chemical_formula_weight         3801.21
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-08-26
_audit_creation_method
;
Olex2 1.2
(compiled 2016.08.23 svn.r3337 for OlexSys, GUI svn.r5217)
;
_audit_update_record
;
2016-08-30 deposited with the CCDC.
2016-10-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   21.6177(6)
_cell_length_b                   21.6177(6)
_cell_length_c                   61.464(4)
_cell_measurement_reflns_used    3748
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      62.509
_cell_measurement_theta_min      2.764
_cell_volume                     24875.4(19)
_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      100.11
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker D8 Venture Photon CMOS'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0689
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       70
_diffrn_reflns_limit_l_min       -65
_diffrn_reflns_number            29562
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        62.509
_diffrn_reflns_theta_max         62.509
_diffrn_reflns_theta_min         2.764
_exptl_absorpt_coefficient_mu    6.658
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_description       Prism
_exptl_crystal_F_000             11628
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.885
_refine_diff_density_min         -0.764
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         4375
_refine_ls_number_restraints     119
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0742
_refine_ls_R_factor_gt           0.0634
_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^)+(0.0745P)^2^+341.5594P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1631
_refine_ls_wR_factor_ref         0.1695
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3748
_reflns_number_total             4375
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce01544a2.cif
_cod_data_source_block           PMBB-2-pcu-1
_cod_original_cell_volume        24875(2)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               7236182
_shelx_estimated_absorpt_t_max   0.349
_shelx_estimated_absorpt_t_min   0.349
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N33-C32
 1.32 with sigma of 0.02
 O31-C32
 1.23 with sigma of 0.02
 O49-C50
 1.23 with sigma of 0.02
 N51-C50
 1.32 with sigma of 0.02
 N51-C53 = N51-C52
 1.45 with sigma of 0.02
 N45-C46 = N45-C47
 1.45 with sigma of 0.02
 N45-C44
 1.32 with sigma of 0.02
 O43-C44
 1.23 with sigma of 0.02
 O31-C36
 1.23 with sigma of 0.02
 N37-C36
 1.32 with sigma of 0.02
 N33-C34 = N33-C35
 1.45 with sigma of 0.02
 O31-C39
 1.23 with sigma of 0.02
 N40-C39
 1.32 with sigma of 0.02
 N40-C41 = N40-C42
 1.45 with sigma of 0.02
 N37-C37 = N37-C38
 1.45 with sigma of 0.02
 N56-C55
 1.32 with sigma of 0.02
 O54-C55
 1.23 with sigma of 0.02
 N56-C57 = N56-C58
 1.45 with sigma of 0.02
 O31-N33
 2.26 with sigma of 0.04
 C32-C35
 2.41 with sigma of 0.04
 O49-N51
 2.26 with sigma of 0.04
 C50-C52
 2.41 with sigma of 0.04
 C50-C53
 2.41 with sigma of 0.04
 C53-C52
 2.47 with sigma of 0.04
 O43-N45
 2.26 with sigma of 0.04
 C44-C47
 2.41 with sigma of 0.04
 C46-C44
 2.41 with sigma of 0.04
 C46-C47
 2.47 with sigma of 0.04
 N37-O31
 2.26 with sigma of 0.04
 C38-C36
 2.41 with sigma of 0.04
 C34-C32
 2.41 with sigma of 0.04
 C34-C35
 2.47 with sigma of 0.04
 N40-O31
 2.26 with sigma of 0.04
 C39-C41
 2.41 with sigma of 0.04
 C39-C42
 2.41 with sigma of 0.04
 C42-C41
 2.47 with sigma of 0.04
 C36-C37
 2.41 with sigma of 0.04
 C38-C37
 2.47 with sigma of 0.04
 O54-N56
 2.26 with sigma of 0.04
 C55-C58
 2.41 with sigma of 0.04
 C57-C55
 2.41 with sigma of 0.04
 C57-C58
 2.47 with sigma of 0.04
3. Restrained planarity
 O49, C50, N51, C52, C53
 with sigma of 0.1
 O43, C44, N45, C46, C47
 with sigma of 0.1
 C32, N33, C34, C35
 with sigma of 0.1
 O31, C39, N40, C41, C42
 with sigma of 0.1
 C36, C37, N37, C38
 with sigma of 0.1
 O54, C55, N56, C57, C58
 with sigma of 0.1
4. Rigid bond restraints
 O31, C32, N33, C34, C35
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O25, C26, N27, C28, C29
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
O49 \\sim C50 \\sim N51 \\sim C52 \\sim C53: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
O31 \\sim C39 \\sim N40 \\sim C41 \\sim C42: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
O31 \\sim C36 \\sim C37 \\sim C38: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
O54 \\sim C55 \\sim N56 \\sim C57 \\sim C58: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
O25 \\sim Cl55: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uiso(C42) = Uiso(C35)
6. Rigid body (RIGU) restrains
 O31, C32, N33, C34, C35
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O25, C26, N27, C28, C29
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Sof(Cl24)=1-FVAR(1)
 Sof(Cl23)=FVAR(1)
 Fixed Sof: O25(0.66667) C26(0.66667) H26(0.66667) N27(0.66667) C28(0.66667)
 H28A(0.66667) H28B(0.66667) H28C(0.66667) C29(0.66667) H29A(0.66667)
 H29B(0.66667) H29C(0.66667) Cl55(0.33333) C32(0.625) H32(0.625) N33(0.625)
 C34(0.625) H34A(0.625) H34B(0.625) H34C(0.625) C35(0.625) H35A(0.625)
 H35B(0.625) H35C(0.625) C36(0.25) H36(0.25) C37(0.25) H37A(0.25) H37B(0.25)
 H37C(0.25) N37(0.25) C38(0.25) H38A(0.25) H38B(0.25) H38C(0.25) C39(0.125)
 H39(0.125) N40(0.125) C41(0.125) H41A(0.125) H41B(0.125) H41C(0.125)
 C42(0.125) H42A(0.125) H42B(0.125) H42C(0.125) O49(0.33333) C50(0.33333)
 H50(0.33333) N51(0.33333) C52(0.33333) H52A(0.33333) H52B(0.33333)
 H52C(0.33333) C53(0.33333) H53A(0.33333) H53B(0.33333) H53C(0.33333)
 O54(0.16666) C55(0.16667) H55(0.16667) N56(0.16667) C57(0.16667) H57A(0.16667)
 H57B(0.16667) H57C(0.16667) C58(0.16667) H58A(0.16667) H58B(0.16667)
 H58C(0.16667) O43(0.33333) C44(0.33333) H44(0.33333) N45(0.33333) C46(0.33333)
 H46A(0.33333) H46B(0.33333) H46C(0.33333) C47(0.33333) H47A(0.33333)
 H47B(0.33333) H47C(0.33333) O48(0.16667)
8.a Riding coordinates:
 C37(H37A,H37B,H37C), C42(H42A,H42B,H42C)
8.b Me refined with riding coordinates:
 C34(H34A,H34B,H34C), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C)
8.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C10(H10), C11(H11), C12(H12), C17(H17), C19(H19), C20(H20), C21(H21),
 C26(H26), C32(H32), C36(H36), C39(H39), C50(H50), C55(H55), C44(H44)
8.d Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C35(H35A,H35B,H35C), C38(H38A,H38B,
 H38C), C41(H41A,H41B,H41C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C46(H46A,
 H46B,H46C), C47(H47A,H47B,H47C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'