Stoichiometry of Adamantylamine-Trinitrophloroglucinol Salts Controlled by Solvate Formation
Smokrović, Kristina; Stilinovic, Vladimir; CrystEngComm  (2020) –; doi:10.1039/C9CE01957J

data_7239821
_publ_section_title
;
 Stoichiometry of Adamantylamine-Trinitrophloroglucinol Salts Controlled
 by Solvate Formation
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C9CE01957J
_journal_year                    2020
_chemical_formula_moiety         '3(C2 H6 O S), C6 N3 O9, 3(C10 H18 N), 2(H2 O)'
_chemical_formula_sum            'C42 H76 N6 O14 S3'
_chemical_formula_weight         985.26
_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   mixed
_audit_creation_date             2018-07-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-07-17 deposited with the CCDC.	2020-01-23 downloaded from the CCDC.
;
_cell_angle_alpha                101.650(4)
_cell_angle_beta                 108.206(5)
_cell_angle_gamma                107.592(5)
_cell_formula_units_Z            2
_cell_length_a                   11.5708(6)
_cell_length_b                   14.8651(9)
_cell_length_c                   17.1263(8)
_cell_measurement_reflns_used    3913
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4300
_cell_measurement_theta_min      4.3860
_cell_volume                     2520.5(3)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            CCD
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega  -20.00   37.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -31.4667   57.0000  -30.0000 57

  2 omega    7.00   80.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       28.6542   77.0000   30.0000 73

  3 omega -100.00  -45.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -31.4667  142.0000 -165.0000 55

  4 omega -113.00  -45.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -31.4667  179.0000    0.0000 68

  5 omega -107.00  -47.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -31.4667  179.0000   30.0000 60

  6 omega  -95.00   40.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -31.4667   19.0000  -30.0000 135

  7 omega -102.00  -35.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -31.4667  -57.0000 -180.0000 67
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_radiation_collimation    0.8
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_unetI/netI     0.0549
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            22839
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.995
_diffrn_reflns_theta_min         4.163
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.214
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90089
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             1060
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.701
_refine_diff_density_min         -0.459
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     635
_refine_ls_number_reflns         10940
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1231
_refine_ls_R_factor_gt           0.0817
_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^)+(0.1088P)^2^+1.6750P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1982
_refine_ls_wR_factor_ref         0.2257
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7108
_reflns_number_total             10940
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce01957j2.cif
_cod_data_source_block           x
_cod_database_code               7239821
_shelx_shelxl_version_number     2016/4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O2-H2A = O2-H2B
 0.85 with sigma of 0.002
 S1-C242 = S1-C241
 1.754 with sigma of 0.00001
 H2AB-H30A
 -1.8 with sigma of 0.02
 H2B-H2A
 1.25 with sigma of 0.04
 H20B-H20C \\sim H20C-H20A
 with sigma of 0.0002
 O301-H30E \\sim O301-H30D
 with sigma of 0.0002
3. Others
 Sof(O2A)=Sof(H2AA)=Sof(H2AB)=1-FVAR(1)
 Sof(O2)=Sof(H2A)=Sof(H2B)=FVAR(1)
4.a Free rotating group:
 O2A(H2AA,H2AB)
4.b Ternary CH refined with riding coordinates:
 C24(H24), C17(H17), C26(H26), C22(H22), C36(H36), C19(H19), C13(H13),
 C34(H34), C32(H32)
4.c Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C28(H28A,H28B), C37(H37A,H37B), C29(H29A,H29B), C11(H11A,
 H11B), C39(H39A,H39B), C12(H12A,H12B), C31(H31A,H31B), C23(H23A,H23B),
 C25(H25A,H25B), C16(H16A,H16B), C33(H33A,H33B), C15(H15A,H15B), C38(H38A,H38B),
  C18(H18A,H18B), C27(H27A,H27B), C14(H14A,H14B), C35(H35A,H35B)
4.d Idealised Me refined as rotating group:
 C220(H22A,H22B,H22C), C221(H22D,H22E,H22F), C230(H23C,H23D,H23E), C231(H23F,
 H23G,H23H), N10(H10A,H10B,H10C), N30(H30A,H30B,H30C), C241(H24A,H24B,H24C),
 C242(H24D,H24E,H24F)
;
_shelx_res_checksum              81056
_olex2_submission_special_instructions 'No special instructions were received'