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_7228218
_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         'C31 H30 Cd N5 O10, C28 H25 Cd N4 O10'
_chemical_formula_sum            'C59 H55 Cd2 N9 O20'
_chemical_formula_weight         1434.92
_space_group_crystal_system      tetragonal
_space_group_IT_number           77
_space_group_name_Hall           'P 4c'
_space_group_name_H-M_alt        'P 42'
_symmetry_space_group_name_Hall  'P 4c'
_symmetry_space_group_name_H-M   'P 42'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-03-10
_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            4
_cell_length_a                   16.984(2)
_cell_length_b                   16.984(2)
_cell_length_c                   21.780(4)
_cell_measurement_reflns_used    260223
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.884
_cell_measurement_theta_min      1.199
_cell_volume                     6282.6(16)
_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 0.997
_diffrn_measured_fraction_theta_max 0.944
_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  0.1306
_diffrn_reflns_av_unetI/netI     0.0507
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            260223
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.939
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         31.888
_diffrn_reflns_theta_min         1.199
_diffrn_source                   'MX1 beamline Australian Synchrotron'
_exptl_absorpt_coefficient_mu    0.758
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_description       block
_exptl_crystal_F_000             2912
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.229
_refine_diff_density_min         -2.675
_refine_diff_density_rms         0.118
_refine_ls_abs_structure_details
;
 Flack x determined using 4315 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.033(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     864
_refine_ls_number_reflns         20299
_refine_ls_number_restraints     154
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1415
_refine_ls_R_factor_gt           0.0883
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2610
_refine_ls_wR_factor_ref         0.3085
_reflns_Friedel_coverage         0.945
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.934
_reflns_number_gt                11169
_reflns_number_total             20299
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce00498b2.cif
_cod_data_source_block           1
_cod_original_cell_volume        6283(2)
_cod_database_code               7228218
_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
 N10-C61 = N10-C62
 1.44 with sigma of 0.01
 C23-C23_$1
 1.45 with sigma of 0.02
 N9-C58 = N9-C59
 1.44 with sigma of 0.01
 N4-C26
 1.32 with sigma of 0.02
 N4-C28 = N4-C27
 1.44 with sigma of 0.01
 N5-C30
 1.44 with sigma of 0.001
 N5-C31
 1.44 with sigma of 0.005
 O20-C60
 1.23 with sigma of 0.02
 O20-H20A = O20-H20B
 0.82 with sigma of 0.001
 O19-H19A = O19-H19B
 0.82 with sigma of 0.001
 C28-C27
 2.5 with sigma of 0.04
 C62-C61
 2.5 with sigma of 0.01
 C59-C58
 2.5 with sigma of 0.04
 C30-C31
 2.5 with sigma of 0.01
 H20A-H20B
 1.3 with sigma of 0.04
 H20A-Cd2
 3 with sigma of 0.04
 H19B-H19A
 1.3 with sigma of 0.04
 H19B-Cd2 = H19A-Cd2
 3 with sigma of 0.04
3. Restrained planarity
 O10, N5, C29, C30, C31
 with sigma of 0.1
 O20, N10, C60, C61, C62
 with sigma of 0.1
 O19, N9, C57, C58, C59
 with sigma of 0.1
4. Rigid bond restraints
 O2, C1, O1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O6, C11, O5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O12, O11, C32
 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(C27) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N4) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C31) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
6. Rigid body (RIGU) restrains
 O9, N4, C26, C27, C28
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O10, N5, C29, C30, C31
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O20, N10, C60, C61, C62
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O19, N9, C57, C58, C59
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Fixed Sof: H19A(0.5) H19B(0.5) H20A(0.5) H20B(0.5) N9(0.5) N10(0.5) C57(0.5)
 H57(0.5) C58(0.5) H58A(0.5) H58B(0.5) H58C(0.5) C59(0.5) H59A(0.5) H59B(0.5)
 H59C(0.5) C60(0.5) H60(0.5) C61(0.5) H61A(0.5) H61B(0.5) H61C(0.5) C62(0.5)
 H62A(0.5) H62B(0.5) H62C(0.5)
8.a Ternary CH refined with riding coordinates:
 C2(H2), C12(H12), C33(H33), C43(H43)
8.b Me refined with riding coordinates:
 C27(H27A,H27B,H27C), C31(H31A,H31B,H31C), C34(H34A,H34B,H34C), C58(H58A,H58B,
 H58C), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C)
8.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C10(H10), C14(H14), C20(H20), C21(H21), C22(H22), C24(H24), C25(H25),
 C26(H26), C29(H29), C35(H35), C41(H41), C47(H47), C51(H51), C52(H52), C53(H53),
  C55(H55), C56(H56), C57(H57), C60(H60)
8.d Idealised Me refined with riding coordinates:
 C59(H59A,H59B,H59C)
8.e Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C13(H13A,H13B,H13C), C28(H28A,H28B,H28C), C30(H30A,H30B,
 H30C), C44(H44A,H44B,H44C)
;
_shelx_res_checksum              29179
_olex2_submission_special_instructions 'No special instructions were received'