A robust metallomacrocyclic motif for the formation interpenetrated coordination polymers
Boer, Stephanie A.; Turner, David R.; CrystEngComm 19 (2017) 2402–; doi:10.1039/C7CE00498B

data_7228214
_publ_section_title
;
 A robust metallomacrocyclic motif for the formation interpenetrated
 coordination polymers
;
_journal_issue                   17
_journal_name_full               CrystEngComm
_journal_page_first              2402
_journal_paper_doi               10.1039/C7CE00498B
_journal_volume                  19
_journal_year                    2017
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C102 H88 Mn4 N14 O38, C3 H7 N O'
_chemical_formula_sum            'C105 H95 Mn4 N15 O39'
_chemical_formula_weight         2410.71
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-03-13
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2017-03-13 deposited with the CCDC.
2017-03-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.324(4)
_cell_length_b                   23.774(5)
_cell_length_c                   14.040(3)
_cell_measurement_reflns_used    102704
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.909
_cell_measurement_theta_min      1.684
_cell_volume                     6116(2)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.7108
_diffrn_reflns_av_R_equivalents  0.0538
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            102704
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.912
_diffrn_reflns_theta_min         1.685
_diffrn_source                   'MX1 beamline Australian Synchrotron'
_exptl_absorpt_coefficient_mu    0.487
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_description       block
_exptl_crystal_F_000             2484
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
TITL 84A_a.res in P2(1)2(1)2
CELL   18.3240   23.7740   14.0400     90.00     90.00     90.00
SPGR P21212
C101 0.086 0.056 0.095 !       2.82 eA-3
C102 0.824 1.001 0.008 !       2.60 eA-3
C103 0.668 0.594 0.662 !       2.57 eA-3
C104 0.950 0.859 0.988 !       2.17 eA-3
C105 0.083 0.061 0.204 !       2.04 eA-3
Q106 0.227 0.749 0.099 !       1.61 eA-3
C107 0.784 0.092 0.160 !       1.52 eA-3
C108 0.062 0.083 0.032 !       1.42 eA-3
Q109 0.713 0.640 0.839 !       1.33 eA-3
C110 0.560 0.407 0.837 !       1.26 eA-3
C111 0.405 0.525 0.787 !       1.12 eA-3
C112 0.068 0.033 0.968 !       1.07 eA-3
C113 0.949 0.936-0.005 !       1.00 eA-3
Q114 0.957 0.159 0.127 !       0.98 eA-3
Q115 0.442 0.636 0.221 !       0.98 eA-3
Q116 0.432 0.227 0.621 !       0.95 eA-3
C117 0.621 0.545 0.838 !       0.78 eA-3
Q118 0.487 0.352 0.341 !       0.78 eA-3
C119 0.644 0.538 0.793 !       0.76 eA-3
Q120 0.297 0.284 0.863 !       0.71 eA-3
Q121 0.626 0.522 0.660 !       0.67 eA-3
C122 0.609 0.509 0.766 !       0.66 eA-3
Q123 0.032 0.951 0.780 !       0.65 eA-3
Q124 0.448 0.564 0.719 !       0.65 eA-3
C125 0.603 0.577 0.748 !       0.63 eA-3
Q126 0.064 0.041 0.887 !       0.59 eA-3
Q127 0.524 0.447 0.268 !       0.58 eA-3
Q128 0.446 0.634 0.768 !       0.58 eA-3
C129 0.611 0.531 0.702 !       0.55 eA-3
Q130 0.892 0.203 0.550 !       0.54 eA-3
C131 0.582 0.508 0.715 !       0.51 eA-3
Q132 0.023 0.768 0.314 !       0.51 eA-3
Q133 0.993 0.149 0.889 !       0.50 eA-3
;
_refine_diff_density_max         1.013
_refine_diff_density_min         -1.045
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details
;
 Flack x determined using 5453 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details                           The solvent assigned from the microanalysis which was not present in the crystal structure (1 DMF and 5.5 H2O molecules) accounts for 95 e- per formula unit.   
;
_refine_ls_abs_structure_Flack   0.033(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     821
_refine_ls_number_reflns         14521
_refine_ls_number_restraints     86
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0581
_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^)+(0.1214P)^2^+3.6823P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1671
_refine_ls_wR_factor_ref         0.1768
_reflns_Friedel_coverage         0.832
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                13071
_reflns_number_total             14521
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce00498b2.cif
_cod_data_source_block           3
_cod_database_code               7228214
_shelx_shelxl_version_number     2016/6
_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, All O(H,H) groups
2. Restrained distances
 N8-C54 = N8-C53
 1.44 with sigma of 0.02
 N9-C55
 1.32 with sigma of 0.01
 O20-C55
 1.23 with sigma of 0.01
 O18B-H18A = O18B-H18B
 0.84 with sigma of 0.02
 O19-H19A = O19-H19B
 0.84 with sigma of 0.02
 H18A-H18B
 1.38 with sigma of 0.04
 H19A-H19B
 1.38 with sigma of 0.04
 H19B-Mn1
 2.5 with sigma of 0.04
 H45-H19B
 2.1 with sigma of 0.04
 Mn2-H18A \\sim Mn2-H18B
 with sigma of 0.02
 Mn1-H19A \\sim Mn1-H19B
 with sigma of 0.02
3. Restrained planarity
 O19, N8, C52, C53, C54
 with sigma of 0.1
4. Rigid bond restraints
 O18A, N7, C49, C50, C51
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O19, N8, C52, C53, C54
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
Uanis(C53) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C42) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O18A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O20) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O18B) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
6. Rigid body (RIGU) restrains
 O20, N9, C55, C56, C57
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Fixed Sof: O18A(0.5) O18B(0.5) H18A(0.5) H18B(0.5) H19A(0.5) H19B(0.5)
 N7(0.5) N8(0.5) C49(0.5) H49(0.5) C50(0.5) H50A(0.5) H50B(0.5) H50C(0.5)
 C51(0.5) H51A(0.5) H51B(0.5) H51C(0.5) C52(0.5) H52(0.5) C53(0.5) H53A(0.5)
 H53B(0.5) H53C(0.5) C54(0.5) H54A(0.5) H54B(0.5) H54C(0.5) O20(0.5) N9(0.5)
 C55(0.5) H55(0.5) C56(0.5) H56A(0.5) H56B(0.5) H56C(0.5) C57(0.5) H57A(0.5)
 H57B(0.5) H57C(0.5)
8.a Ternary CH refined with riding coordinates:
 C2(H2), C12(H12), C22(H22), C32(H32)
8.b Me refined with riding coordinates:
 C50(H50A,H50B,H50C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C56(H56A,H56B,
 H56C), C57(H57A,H57B,H57C)
8.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C10(H10), C16(H16), C20(H20), C26(H26), C30(H30), C36(H36), C40(H40),
 C41(H41), C42(H42), C44(H44), C45(H45), C46(H46), C49(H49), C52(H52), C55(H55)
8.d Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C13(H13A,H13B,H13C), C23(H23A,H23B,H23C), C33(H33A,H33B,
 H33C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C51(H51A,H51B,H51C)
;
_shelx_res_checksum              47327
_shelx_fab_checksum              22943
_olex2_submission_special_instructions 'No special instructions were received'