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_7244209
_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 N5 Zn, 1.5(F6 P), F2.588 P0.5, 0.412(F)'
_chemical_formula_sum            'C10 H25 F12 N5 P2 Zn'
_chemical_formula_weight         570.66
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_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                90
_cell_angle_beta                 106.102(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.6817(10)
_cell_length_b                   25.670(3)
_cell_length_c                   12.8729(10)
_cell_measurement_reflns_used    9913
_cell_measurement_temperature    150
_cell_measurement_theta_max      31.1715
_cell_measurement_theta_min      3.1550
_cell_volume                     4026.2(7)
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_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  0.0634
_diffrn_reflns_av_unetI/netI     0.0528
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            26484
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         31.167
_diffrn_reflns_theta_min         2.175
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    1.887
_exptl_absorpt_correction_T_max  0.9281
_exptl_absorpt_correction_T_min  0.6732
_exptl_absorpt_process_details
;
SADABS v2014.5 (Sheldrick)
Estimated minimum and maximum transmission:  0.6732  0.9281
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.883
_exptl_crystal_description       block
_exptl_crystal_F_000             2304
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.340
_refine_diff_density_min         -0.628
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         5002
_refine_ls_number_restraints     246
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0628
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0972P)^2^+12.3968P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1758
_refine_ls_wR_factor_ref         0.1896
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3898
_reflns_number_total             5002
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01534f2.cif
_cod_data_source_block           je07
_cod_depositor_comments
'Adding full bibliography for 7244202--7244217.cif.'
_cod_database_code               7244209
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.946
_shelx_estimated_absorpt_t_min   0.928
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.98854
 0.01146
2. Restrained distances
 P1-F1 = P1-F2 = P1-F3 = P1-F4 = P1-F5 = P1-F6
 1.595 with sigma of 0.02
 P3-F11 = P3-F12 = P3-F13 = P3-F14 = P3-F13A = P3-F16
 1.595 with sigma of 0.02
 P3-F12A = P3-F13A
 1.595 with sigma of 0.02
 F11-F12 = F12-F13 = F13-F14 = F14-F11
 2.256 with sigma of 0.02
 F16-F11 = F16-F12 = F16-F13 = F16-F14
 2.256 with sigma of 0.02
 F12A-F13A = F12A-F12A_$1
 2.256 with sigma of 0.02
 P2-F9A \\sim P2-F8 \\sim P2-F10 \\sim P2-F9 \\sim P2-F7 \\sim P2-F10A
 with sigma of 0.02
 F9A-F10A \\sim F8-F9 \\sim F10-F9
 with sigma of 0.04
 P2-F9 \\sim P2-F9A
 with sigma of 0.02
 P2-F10 \\sim P2-F10A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
F16 \\sim F13A \\sim F13 \\sim F12 \\sim F12A \\sim F14 \\sim F11: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
P2 \\sim F9 \\sim F10A \\sim F10 \\sim F7 \\sim F9A \\sim F8: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
F9 \\sim F10 \\sim F8: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
Uanis(F4) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F3) \\sim
Ueq, Uanis(F5) \\sim Ueq, Uanis(F1) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(P2) \\sim Ueq, Uanis(F10A) \\sim Ueq, Uanis(F7) \\sim Ueq, Uanis(F9A)
\\sim Ueq, : with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Rigid body (RIGU) restrains
 P3, F16, F13A, F13, F12, F12A, F14, F11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F13A)=Sof(F12A)=1-FVAR(1)
 Sof(F11)=Sof(F12)=Sof(F13)=Sof(F14)=0.5*FVAR(2)
 Sof(F9A)=Sof(F10A)=1-FVAR(2)
 Sof(F8)=Sof(F10)=0.5*FVAR(3)
 Sof(F9)=FVAR(2)
6.a Riding coordinates:
 N1(H1), N3(H3), N5(H5)
6.b Ternary CH refined with riding coordinates:
 N2(H2), N4(H4)
6.c 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)
;
_shelx_res_checksum              22262
_shelx_hkl_checksum              52914
_olex2_submission_special_instructions 'No special instructions were received'