Design and synthesis of nucleobase-incorporated metal‒organic materials
Zhang, Muwei; Lu, Weigang; Li, Jian-Rong; Bosch, Mathieu; Chen, Ying-Pin; Liu, Tian-Fu; Liu, Yangyang; Zhou, Hong-Cai; Inorganic Chemistry Frontiers 1 (2014) 159–; doi:10.1039/c3qi00042g

data_4350739
_publ_section_title
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 Design and synthesis of nucleobase-incorporated metal--organic materials
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_journal_issue                   2
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              159
_journal_paper_doi               10.1039/c3qi00042g
_journal_volume                  1
_journal_year                    2014
_chemical_formula_moiety         'C184 H156 Cu12 N28 O84'
_chemical_formula_sum            'C184 H156 Cu12 N28 O84'
_chemical_formula_weight         4865.85
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-09-20
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_cell_angle_alpha                109.319(2)
_cell_angle_beta                 106.426(2)
_cell_angle_gamma                107.1820(10)
_cell_formula_units_Z            2
_cell_length_a                   27.990(3)
_cell_length_b                   28.102(3)
_cell_length_c                   28.303(5)
_cell_measurement_reflns_used    71236
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      1.68
_cell_volume                     18196(4)
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
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SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      110.15
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0761
_diffrn_reflns_av_unetI/netI     0.1574
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            190892
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.68
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.744
_exptl_absorpt_correction_T_max  0.8077
_exptl_absorpt_correction_T_min  0.7075
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            blue-green
_exptl_crystal_density_diffrn    0.888
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4952.0
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.3
_platon_squeeze_details
;
;
_refine_diff_density_max         2.219
_refine_diff_density_min         -1.620
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2158
_refine_ls_number_reflns         71236
_refine_ls_number_restraints     171
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.1691
_refine_ls_R_factor_gt           0.1014
_refine_ls_shift/su_max          0.099
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1200P)^2^+12.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2622
_refine_ls_wR_factor_ref         0.2841
_reflns_number_gt                27200
_reflns_number_total             71236
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3qi00042g.txt
_cod_data_source_block           tmop_p-1_sq
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
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_cod_database_code               4350739
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N10-C11 = C11-N12 = N12-C13 = C13-C14 = C14-C15
 1.39 with sigma of 0.002
 N10-N12 = N12-C14 = C14-N10 = C13-C15
 2.408 with sigma of 0.003
 C16-C14
 1.508 with sigma of 0.002
 C16-C13 = C16-C15
 2.5 with sigma of 0.002
 C49-N50 = C49B-N50B
 1.45 with sigma of 0.002
 N50-C51 = C51-N52 = N52-C53 = C53-C54 = C54-C55
 1.39 with sigma of 0.002
 N50-N52 = N52-C54 = C54-N50 = C53-C55
 2.408 with sigma of 0.003
 C56-C54
 1.508 with sigma of 0.002
 C56-C53 = C56-C55
 2.5 with sigma of 0.002
 N50B-C51B = C51B-N52B = N52B-C53B = C53B-C54B = C54B-C55B
 1.39 with sigma of 0.002
 N50B-N52B = N52B-C54B = C54B-N50B = C53B-C55B
 2.408 with sigma of 0.003
 C56B-C54B
 1.508 with sigma of 0.002
 C56B-C53B = C56B-C55B
 2.5 with sigma of 0.002
 O18B-C54B
 2.1 with sigma of 0.002
 N70-C71 = N70-C75 = N72-C71 = N72-C73
 1.35 with sigma of 0.002
 C74-C73 = C74-C75
 1.39 with sigma of 0.002
 C74-N70 = C74-N72 = C75-C73 = C75-C71
 2.408 with sigma of 0.002
 C76-C73 = C76-C75
 2.5 with sigma of 0.002
 C76-C74
 1.508 with sigma of 0.002
 O23-N70 = O24-N72
 2.1 with sigma of 0.002
 N110-C111 = N110-C115 = N112-C111 = N112-C113
 1.35 with sigma of 0.002
 C114-C113 = C114-C115
 1.39 with sigma of 0.002
 C114-N110 = C114-N112 = C115-C113 = C115-C111
 2.408 with sigma of 0.002
 N310-C311 = N310-C315 = N312-C311 = N312-C313
 1.35 with sigma of 0.002
 C314-C313 = C314-C315
 1.39 with sigma of 0.002
 C314-N310 = C314-N312 = C315-C313 = C315-C311
 2.408 with sigma of 0.002
 C116-C114 = C316-C314
 1.508 with sigma of 0.002
 C311-O35B = C313-O36B
 1.28 with sigma of 0.002
 C103-C104 = C105-C106 = C107-C108
 1.39 with sigma of 0.001
 C103-C105 = C105-C107 = C104-C106
 2.408 with sigma of 0.001
 C303-C304 = C305-C306 = C307-C308
 1.39 with sigma of 0.001
 C303-C305 = C305-C307 = C304-C306
 2.408 with sigma of 0.001
 N150-C151 = N150-C155 = N152-C151 = N152-C153
 1.35 with sigma of 0.002
 C154-C153 = C154-C155
 1.39 with sigma of 0.002
 C154-N150 = C154-N152 = C155-C153 = C155-C151
 2.408 with sigma of 0.002
 C156-C153 = C156-C155
 2.5 with sigma of 0.002
 C156-C154
 1.508 with sigma of 0.002
 O47-N152 = O48-N152
 2.1 with sigma of 0.002
 C149-N150
 1.45 with sigma of 0.003
 N230-C231 = N230-C235 = N232-C231 = N232-C233
 1.35 with sigma of 0.002
 C234-C233 = C234-C235
 1.39 with sigma of 0.002
 C234-N230 = C234-N232 = C235-C233 = C235-C231
 2.408 with sigma of 0.002
 C236-C233 = C236-C235
 2.5 with sigma of 0.002
 C236-C234
 1.508 with sigma of 0.002
 C226-C229
 1.49 with sigma of 0.003
 C229-N230
 1.45 with sigma of 0.003
3. Restrained planarity
 C9, N10, C11, N12, C13, C14, C15, C16, O5, O6
 with sigma of 0.001
 C49, N50, C51, N52, C53, C54, C55, C56, O17, O18
 with sigma of 0.001
 C49B, N50B, C51B, N52B, C53B, C54B, C55B, C56B, O17B, O18B
 with sigma of 0.001
 C103, C104, C105, C106, C107, C108, C109
 with sigma of 0.001
 C109, N110, C111, N112, C113, C114, C115, C116, O35, O36
 with sigma of 0.001
 C309, N310, C311, N312, C313, C314, C315, C316, O35B, O36B
 with sigma of 0.001
 C103, C104, C105, C106, C107, C108
 with sigma of 0.001
 C303, C104, C305, C306, C307, C108
 with sigma of 0.001
 C229, N230, C231, N232, C233, C234, C235, C236
 with sigma of 0.001
4. Uiso/Uaniso restraints and constraints
Uanis(N10) = Uanis(C11) = Uanis(N12) = Uanis(C13) = Uanis(C14) = Uanis(C15) =
Uanis(C16) = Uanis(O5) = Uanis(O6)
Uanis(C49) = Uanis(N50) = Uanis(C51) = Uanis(N52) = Uanis(C53) = Uanis(C54) =
Uanis(C55) = Uanis(C56) = Uanis(O17) = Uanis(O18) = Uanis(C49B) = Uanis(N50B) =
Uanis(C51B) = Uanis(N52B) = Uanis(C53B) = Uanis(C54B) = Uanis(C55B) =
Uanis(C56B) = Uanis(O17B) = Uanis(O18B)
Uanis(C69) = Uanis(N70) = Uanis(C71) = Uanis(N72) = Uanis(C73) = Uanis(C74) =
Uanis(C75) = Uanis(C76) = Uanis(O23) = Uanis(O24) = Uanis(C63) = Uanis(C64) =
Uanis(C65) = Uanis(C66) = Uanis(C67) = Uanis(C68)
Uanis(C309) = Uanis(N310) = Uanis(C311) = Uanis(N312) = Uanis(C313) =
Uanis(C314) = Uanis(C315) = Uanis(C316) = Uanis(O35B) = Uanis(O36B) =
Uanis(C109) = Uanis(N110) = Uanis(C111) = Uanis(N112) = Uanis(C113) =
Uanis(C114) = Uanis(C115) = Uanis(C116) = Uanis(O35) = Uanis(O36)
Uanis(C303) = Uanis(C304) = Uanis(C305) = Uanis(C306) = Uanis(C307) =
Uanis(C308)
Uanis(C149) = Uanis(N150) = Uanis(C151) = Uanis(N152) = Uanis(C153) =
Uanis(C154) = Uanis(C155) = Uanis(C156) = Uanis(O47) = Uanis(O48) = Uanis(C143)
= Uanis(C144) = Uanis(C145) = Uanis(C146) = Uanis(C147) = Uanis(C148)
Uanis(C229) = Uanis(N230) = Uanis(C231) = Uanis(N232) = Uanis(C233) =
Uanis(C234) = Uanis(C235) = Uanis(C236) = Uanis(O71) = Uanis(O72) = Uanis(C223)
= Uanis(C224) = Uanis(C225) = Uanis(C226) = Uanis(C227) = Uanis(C228)
Uanis(O2S) = Uanis(C1S) = Uanis(C2S) = Uanis(C3S) = Uanis(N4S) = Uanis(C5S)
Uanis(O4S) = Uanis(C6S) = Uanis(C7S) = Uanis(N8S) = Uanis(C9S) = Uanis(C10S)
Uanis(O8S) = Uanis(C11S) = Uanis(C12S) = Uanis(C13S) = Uanis(N14S) = Uanis(C15S)
Uanis(O10S) = Uanis(C16S) = Uanis(C17S) = Uanis(N18S) = Uanis(C19S) =
Uanis(C20S)
5. Others
 Sof(C49B)=Sof(H49C)=Sof(H49D)=Sof(N50B)=Sof(C51B)=Sof(N52B)=Sof(H52B)=
 Sof(C53B)=Sof(C54B)=Sof(C55B)=Sof(H55B)=Sof(C56B)=Sof(H56D)=Sof(H56E)=
 Sof(H56F)=Sof(O17B)=Sof(O18B)=1-FVAR(1)
 Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(N50)=Sof(C51)=Sof(N52)=Sof(H52)=Sof(C53)=
 Sof(C54)=Sof(C55)=Sof(H55)=Sof(C56)=Sof(H56A)=Sof(H56B)=Sof(H56C)=Sof(O17)=
 Sof(O18)=FVAR(1)
 Sof(C303)=Sof(H303)=Sof(C304)=Sof(C305)=Sof(H305)=Sof(C306)=Sof(C307)=
 Sof(H307)=Sof(C308)=Sof(C309)=Sof(H30A)=Sof(H30B)=Sof(N310)=Sof(C311)=
 Sof(N312)=Sof(H312)=Sof(C313)=Sof(C314)=Sof(C315)=Sof(H315)=Sof(C316)=
 Sof(H31A)=Sof(H31B)=Sof(H31C)=Sof(O35B)=Sof(O36B)=1-FVAR(2)
 Sof(C103)=Sof(H103)=Sof(C104)=Sof(C105)=Sof(H105)=Sof(C106)=Sof(C107)=
 Sof(H107)=Sof(C108)=Sof(C109)=Sof(H10A)=Sof(H10B)=Sof(N110)=Sof(C111)=
 Sof(N112)=Sof(H112)=Sof(C113)=Sof(C114)=Sof(C115)=Sof(H115)=Sof(C116)=
 Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(O35)=Sof(O36)=FVAR(2)
6.a Riding coordinates:
 C3S(H3SA,H3SB,H3SC), C5S(H5SA,H5SB,H5SC)
6.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C29(H29A,H29B), C49(H49A,H49B), C49B(H49C,H49D), C69(H69A,H69B),
 C89(H89A,H89B), C109(H10A,H10B), C309(H30A,H30B), C129(H12A,H12B), C149(H14A,
 H14B), C169(H16D,H16E), C189(H18A,H18B), C209(H20A,H20B), C229(H22A,H22B)
6.c Me refined with riding coordinates:
 C16(H16A,H16B,H16C), C36(H36A,H36B,H36C), C56(H56A,H56B,H56C), C56B(H56D,H56E,
 H56F), C76(H76A,H76B,H76C), C96(H96A,H96B,H96C), C116(H11A,H11B,H11C),
 C316(H31A,H31B,H31C), C136(H13A,H13B,H13C), C156(H15A,H15B,H15C), C176(H17A,
 H17B,H17C), C196(H19A,H19B,H19C), C216(H21A,H21B,H21C), C236(H23A,H23B,H23C),
 C6S(H6SA,H6SB,H6SC), C9S(H9SA,H9SB,H9SC), C10S(H10C,H10D,H10E), C11S(H11D,H11E,
 H11F), C13S(H13D,H13E,H13F), C15S(H15D,H15E,H15F), C16S(H16F,H16G,H16H),
 C19S(H19D,H19E,H19F), C20S(H20C,H20D,H20E)
6.d Aromatic/amide H refined with riding coordinates:
 N12(H12), N32(H32), N72(H72), N92(H92), N132(H132), N152(H152), N172(H172),
 N192(H192), N212(H212), N232(H232), C3(H3), C5(H5), C7(H7), C15(H15), C23(H23),
  C25(H25), C27(H27), C35(H35), C43(H43), C45(H45), C47(H47), N52(H52),
 C55(H55), N52B(H52B), C55B(H55B), C63(H63), C65(H65), C67(H67), C75(H75),
 C83(H83), C85(H85), C87(H87), C95(H95), C103(H103), C105(H105), C107(H107),
 N112(H112), C115(H115), C303(H303), C305(H305), C307(H307), N312(H312),
 C315(H315), C123(H123), C125(H125), C127(H127), C135(H135), C143(H143),
 C145(H145), C147(H147), C155(H155), C163(H163), C165(H165), C167(H167),
 C175(H175), C183(H183), C185(H185), C187(H187), C195(H195), C204(H204),
 C206(H206), C208(H208), C215(H215), C223(H223), C225(H225), C227(H227),
 C235(H235)
6.e Fitted hexagon refined as free rotating group:
 C3(C4,C5,C6,C7,C8), C23(C24,C25,C26,C27,C28), C43(C44,C45,C46,C47,C48),
 C63(C64,C65,C66,C67,C68), C83(C84,C85,C86,C87,C88), C103(C104,C105,C106,C107,
 C108), C303(C304,C305,C306,C307,C308), C123(C124,C125,C126,C127,C128),
 C143(C144,C145,C146,C147,C148), C163(C164,C165,C166,C167,C168), C183(C184,C185,
 C186,C187,C188), C203(C204,C205,C206,C207,C208), C223(C224,C225,C226,C227,C228)
6.f Idealised Me refined as rotating group:
 C1S(H1SA,H1SB,H1SC)
;