Expanding and quantifying the crystal chemistry of the flexible ligand 15aneN5
Shircliff, Anthony D.; Allbritton, Elisabeth M. A.; Davilla, Dustin J.; Gorbet, Michael-Joseph; Jones, Donald G.; Tresp, David S.; Allen, Michael B.; Shrestha, Alina; Burgess, Gwendolyn E.; Eze, John I.; Fernandez, Andrea T.; Ramirez, Daniel; Shoff, Kody J.; Crispin, Garet G.; Crone, Sarah B.; Flinn, Michael; Tran, Tien; Bryce, Darby S.; Bond, Abbagale L.; Shockey, Dylan W.; Oliver, Allen G.; Krause, Jeanette A.; Prior, Timothy J.; Hubin, Timothy J.; CrystEngComm 24 (2022) 1218–1236; doi:10.1039/D1CE01534F

data_7244210
_publ_section_title
;
 Expanding and quantifying the crystal chemistry of the flexible ligand
 15aneN5
;
_journal_issue                   6
_journal_name_full               CrystEngComm
_journal_page_first              1218
_journal_page_last               1236
_journal_paper_doi               10.1039/D1CE01534F
_journal_volume                  24
_journal_year                    2022
_chemical_formula_moiety         'C10 H25 Cl Cr N5, Cl, 1(F6 P)'
_chemical_formula_sum            'C10 H25 Cl2 Cr F6 N5 P'
_chemical_formula_weight         483.22
_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     dual
_audit_creation_date             2021-07-22
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-08-04 deposited with the CCDC.	2022-01-04 downloaded from the CCDC.
;
_cell_angle_alpha                97.589(3)
_cell_angle_beta                 93.469(2)
_cell_angle_gamma                96.344(2)
_cell_formula_units_Z            4
_cell_length_a                   9.0957(8)
_cell_length_b                   9.2333(9)
_cell_length_c                   22.464(2)
_cell_measurement_reflns_used    9869
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      31.053
_cell_measurement_theta_min      2.444
_cell_volume                     1853.2(3)
_computing_cell_refinement       'Bruker SAINT v8.37A'
_computing_data_collection       'Bruker APEX3 v2016.1.0'
_computing_data_reduction        'Bruker SAINT v8.37A'
_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)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker PHOTON100 CMOS'
_diffrn_measurement_method       'omega-phi scans'
_diffrn_radiation_monochromator  'Si-<111> channel cut crystal'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0462
_diffrn_reflns_av_unetI/netI     0.0437
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            36477
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         31.094
_diffrn_reflns_theta_min         2.444
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    1.334
_exptl_absorpt_correction_T_max  0.9281
_exptl_absorpt_correction_T_min  0.8161
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2014/5  0.8161  0.9281'
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.732
_exptl_crystal_description       block
_exptl_crystal_F_000             988
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.025
_exptl_crystal_size_min          0.015
_refine_diff_density_max         0.787
_refine_diff_density_min         -0.465
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     497
_refine_ls_number_reflns         9167
_refine_ls_number_restraints     205
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0453
_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^)+(0.0438P)^2^+2.3863P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1058
_refine_ls_wR_factor_ref         0.1122
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7339
_reflns_number_total             9167
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01534f2.cif
_cod_data_source_block           dgj07bp-1
_cod_depositor_comments
'Adding full bibliography for 7244202--7244217.cif.'
_cod_database_code               7244210
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.980
_shelx_estimated_absorpt_t_min   0.949
_olex2_refinement_description
;
1. Restrained distances
 P2-F6 \\sim P2-F6A
 with sigma of 0.02
 P2-F9 \\sim P2-F9A
 with sigma of 0.02
 P2-F10 \\sim P2-F10A
 with sigma of 0.02
 P2-F11 \\sim P2-F11A
 with sigma of 0.02
 P2-F12 \\sim P2-F12A
 with sigma of 0.02
 P2-F9 \\sim P2-F12 \\sim P2-F10A \\sim P2-F10 \\sim P2-F8 \\sim P2-F6A \\sim
P2-F6 \\sim P2-F11 \\sim P2-F9A
 \\sim P2-F11A \\sim P2-F12A
 with sigma of 0.02
 F9-F12 \\sim F9-F10 \\sim F9-F6 \\sim F12-F10 \\sim F12-F6 \\sim F12-F11 \\sim
F10A-F9A \\sim F10A-F11A ~
 F10A-F12A \\sim F10-F11 \\sim F6A-F9A \\sim F6A-F11A \\sim F6A-F12A \\sim
F6-F11 \\sim F9A-F12A \\sim F11A-
 F12A
 with sigma of 0.04
2. Uiso/Uaniso restraints and constraints
F12A \\sim F12: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
F11A \\sim F11: within 2A with sigma of 0.0125 and sigma for terminal atoms of
0.04 within 2A
F9A \\sim F9: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
F10 \\sim F10A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
F6A \\sim F6: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
3. Others
 Sof(F6A)=Sof(F11A)=Sof(F9A)=Sof(F10A)=Sof(F12A)=1-FVAR(1)
 Sof(F6)=Sof(F9)=Sof(F10)=Sof(F11)=Sof(F12)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 N1(H1), N2(H2), N3(H3), N4(H4), N5(H5), N6(H6), N7(H7), N8(H8), N9(H9),
 N10(H10)
4.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B),
  C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B)
;
_shelx_res_checksum              68610
_shelx_hkl_checksum              15655
_olex2_submission_special_instructions 'No special instructions were received'