Structure and performance regulation of energetic complexes through multifunctional molecular self-assembly.
Dong, Wen-Shuai; Mei, Hao-Zheng; Yu, Qi-Yao; Xu, Mei-Qi; Li, Zong-You; Zhang, Jian-Guo; Dalton transactions (Cambridge, England : 2003) 53 (2024) 13925–13932; doi:10.1039/d4dt00830h

data_7716759
_publ_section_title
;
 Structure and performance regulation of energetic complexes through
 multifunctional molecular self-assembly.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13925
_journal_page_last               13932
_journal_paper_doi               10.1039/d4dt00830h
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety
'7(C3 H18 Mn N12 O3), C3 H17 Mn N12 O3, 6(C2 N4 O8), 5[H2O]'
_chemical_formula_sum            'C36 H153 Mn8 N120 O77'
_chemical_formula_weight         3938.87
_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_Hall           'R 3'
_space_group_name_H-M_alt        'R 3 :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2024-07-18
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2024-07-19 deposited with the CCDC.	2024-07-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            9
_cell_length_a                   36.583(3)
_cell_length_b                   36.583(3)
_cell_length_c                   28.975(3)
_cell_measurement_reflns_used    3448
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.458
_cell_measurement_theta_min      3.067
_cell_volume                     33582(5)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1132
_diffrn_reflns_av_unetI/netI     0.2081
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            54652
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.016
_diffrn_reflns_theta_max         25.016
_diffrn_reflns_theta_min         1.840
_exptl_absorpt_coefficient_mu    0.787
_exptl_absorpt_correction_T_max  0.9470
_exptl_absorpt_correction_T_min  0.7703
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.713
_exptl_crystal_description       neddle
_exptl_crystal_F_000             17775
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.836
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details
;
 Flack x determined using 2492 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.886
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1808
_refine_ls_number_reflns         26173
_refine_ls_number_restraints     7518
_refine_ls_restrained_S_all      0.825
_refine_ls_R_factor_all          0.2089
_refine_ls_R_factor_gt           0.1007
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1093P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2252
_refine_ls_wR_factor_ref         0.2720
_reflns_Friedel_coverage         0.985
_reflns_Friedel_fraction_full    0.984
_reflns_Friedel_fraction_max     0.984
_reflns_number_gt                9075
_reflns_number_total             26173
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00830h2.cif
_cod_data_source_block           200827h_sq
_cod_depositor_comments
'Adding full bibliography for 7716752--7716760.cif.'
_cod_original_cell_volume        33582(7)
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               7716759
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.947
_shelx_estimated_absorpt_t_min   0.770
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H) groups, {H6A,H6B} of N6, {H10A,H10B} of N10, {H2A,H2B} of N2,
  {H14A,H14B} of N14, {H26A,H26B} of N26, {H42A,H42B} of N42, {H18A,H18B} of
  N18, {H30A,H30B} of N30, {H40A,H40B} of N40, {H38A,H38B} of N38, {H34A,H34B}
  of N34, {H22A,H22B} of N22, {H46A,H46B} of N46, {H54A,H54B} of N54, {H50A,
  H50B} of N50, {H62A,H62B} of N62, {H58A,H58B} of N58, {H66A,H66B} of N66,
  {H70A,H70B} of N70, {H74A,H74B} of N74, {H82A,H82B} of N82, {H94A,H94B} of
  N94, {H86A,H86B} of N86, {H78A,H78B} of N78, {H84A,H84B} of N84, {H90A,H90B}
  of N90, All N(H,H,H) groups
 At 1.5 times of:
  {H8A,H8B} of N8, {H4A,H4B} of N4, {H16A,H16B} of N16, {H12A,H12B} of N12,
  {H20A,H20B} of N20, {H24A,H24B} of N24, {H32A,H32B} of N32, {H36A,H36B} of
  N36, {H56A,H56B} of N56, {H64A,H64B} of N64, {H68A,H68B} of N68, {H52A,H52B}
  of N52, {H48A,H48B} of N48, {H60A,H60B} of N60, {H44A,H44B} of N44, {H72A,
  H72B} of N72, {H88A,H88B} of N88, {H92A,H92B} of N92, {H96A,H96B} of N96,
  {H76A,H76B} of N76, {H80A,H80B} of N80
2. Restrained distances
 C11-O11
 1.32 with sigma of 0.01
 C11-N41 = C11-N43 = C12-N47 = C24-N95 = C7-N27 = C18-N71
 1.42 with sigma of 0.01
 N41-N42 = N43-N44 = N47-N48 = N95-N96 = N27-N28
 1.37 with sigma of 0.01
 C11-N44 = C12-N48 = C24-N96 = C7-N28
 2.43 with sigma of 0.002
 H59-H81
 2.3 with sigma of 0.02
3. Rigid bond restraints
 N27, N28
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.001
 O11, C11, N71, C18, N95, C24, N99, C26, O48, N108, N19, N20, N43, N44
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.001
 O45, N107
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 3.8A with sigma of 0.02 and sigma
for terminal atoms of 0.04 within 3.8A
5. Others
 Fixed Sof: H28B(0.5) H28C(0.5)
6.a Riding coordinates:
 N4(H4A,H4B), N8(H8A,H8B), N12(H12A,H12B), N16(H16A,H16B), N20(H20A,H20B),
 N24(H24A,H24B), N28(H28A,H28B,H28C), N32(H32A,H32B), N36(H36A,H36B), N40(H40A,
 H40B), N44(H44A,H44B), N48(H48A,H48B), N52(H52A,H52B), N56(H56A,H56B),
 N60(H60A,H60B), N64(H64A,H64B), N68(H68A,H68B), N72(H72A,H72B), N76(H76A,H76B),
  N80(H80A,H80B), N88(H88A,H88B), N92(H92A,H92B), N96(H96A,H96B)
6.b :
 O1(O2,O3,O4,O5,O6,O7,O8,O9,O10,O11,O12,O13,O14,O15,O16,O17,O18,O19,O20,O21,
 O22,O23,O24,O25,O26,O27,O28,O29,O30,O31,O32,O33,O34,O35,O36,O37,O38,O39,O40,
 O41,O42,O43,O44,O45,O46,O47,O48,O49,O50,O51,O52,O53,O54,O55,O56,O57,O58,O59,
 O60,O61,O62,O63,O64,O65,O66,O67,O68,O69,O70,O71,O72,C1,C2,C3,C4,C5,C6,C7,C8,C9,
 C10,C11,C12,C13,C14,C15,C16,C17,C18,C19,C20,C21,C22,C23,C24,C25,C26,C27,C28,
 C29,C30,C31,C32,C33,C34,C35,C36)
6.c Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), N6(H6A,H6B), N10(H10A,H10B), N14(H14A,H14B), N18(H18A,H18B),
 N22(H22A,H22B), N26(H26A,H26B), N30(H30A,H30B), N34(H34A,H34B), N38(H38A,H38B),
  N42(H42A,H42B), N46(H46A,H46B), N50(H50A,H50B), N54(H54A,H54B), N58(H58A,
 H58B), N62(H62A,H62B), N66(H66A,H66B), N70(H70A,H70B), N74(H74A,H74B),
 N78(H78A,H78B), N82(H82A,H82B), N86(H86A,H86B), N90(H90A,H90B), N94(H94A,H94B)
6.d Aromatic/amide H refined with riding coordinates:
 N1(H1), N3(H3), N5(H5), N7(H7), N9(H9), N11(H11), N13(H13), N15(H15),
 N17(H17), N19(H19), N21(H21), N23(H23), N25(H25), N27(H27), N29(H29), N31(H31),
  N33(H33), N35(H35), N37(H37), N39(H39), N41(H41), N43(H43), N45(H45),
 N47(H47), N49(H49), N51(H51), N53(H53), N55(H55), N59(H59), N61(H61), N63(H63),
  N65(H65), N67(H67), N69(H69), N71(H71), N73(H73), N75(H75), N77(H77),
 N79(H79), N81(H81), N83(H83), N85(H85), N87(H87), N89(H89), N91(H91), N93(H93),
  N95(H95)
6.e X=CH2 refined with riding coordinates:
 N84(H84A,H84B)
;
_shelx_res_checksum              61791
_shelx_hkl_checksum              75575
_shelx_fab_checksum              68820
_platon_squeeze_special_details
;
A solvent mask was calculated and 474 electrons were
found in a volume of 2740\%A^3 in 10 voids per unit cell.
This is consistent with the presence of 
5[H2O] per Asymmetric Unit 
which account for 450 electrons 
per unit cell.
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'