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_7244214
_publ_section_title
;
 Expanding and quantifying the crystal chemistry of the flexible ligand
 15aneN5
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_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_absolute_configuration ad
_chemical_formula_moiety         'C10 H25 Cu N5, 2(F6 P), 2(C H3 N O2)'
_chemical_formula_sum            'C12 H31 Cu F12 N7 O4 P2'
_chemical_formula_weight         690.92
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 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                90
_cell_angle_beta                 104.977(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.2222(4)
_cell_length_b                   12.5513(7)
_cell_length_c                   12.9958(7)
_cell_measurement_reflns_used    9873
_cell_measurement_temperature    150
_cell_measurement_theta_max      31.078
_cell_measurement_theta_min      2.8965
_cell_volume                     1295.60(12)
_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 0.997
_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  0.0511
_diffrn_reflns_av_unetI/netI     0.0572
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            47487
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         31.093
_diffrn_reflns_theta_min         1.769
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    1.372
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6738
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 
 Estimated minimum and maximum transmission:  0.6738  0.7462
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.771
_exptl_crystal_description       plate
_exptl_crystal_F_000             702
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.646
_refine_diff_density_min         -0.604
_refine_diff_density_rms         0.171
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.44(9)
_refine_ls_extinction_coef       0.033(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     458
_refine_ls_number_reflns         6354
_refine_ls_number_restraints     754
_refine_ls_restrained_S_all      1.188
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0355
_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^)+(0.0388P)^2^+0.2256P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0699
_refine_ls_wR_factor_ref         0.0702
_reflns_Friedel_coverage         0.906
_reflns_Friedel_fraction_full    0.986
_reflns_Friedel_fraction_max     0.987
_reflns_number_gt                6278
_reflns_number_total             6354
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01534f2.cif
_cod_data_source_block           ks11
_cod_depositor_comments
'Adding full bibliography for 7244202--7244217.cif.'
_cod_database_code               7244214
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.966
_shelx_estimated_absorpt_t_min   0.922
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.55926
 0.44074
2. Restrained distances
 N3-C5 \\sim N3-C5A
 with sigma of 0.02
 N4-C5 \\sim N4-C5A
 with sigma of 0.04
 N4-C6 \\sim N4-C6A
 with sigma of 0.02
 C5-C6 \\sim C5A-C6A
 with sigma of 0.02
 N3-C6 \\sim N3-C6A
 with sigma of 0.04
 F8-F9 \\sim F8-F12 \\sim F9-F11 \\sim F11-F12 \\sim F12A-F8A \\sim F12A-F11A
\\sim F8A-F9A \\sim F9A-F11A
 with sigma of 0.04
 P1-F1 \\sim P1-F2 \\sim P1-F3 \\sim P1-F4 \\sim P1-F5 \\sim P1-F6 \\sim P1-F6A
\\sim P1-F5A \\sim P1-F1A \\sim P1-
 F3A \\sim P1-F2A \\sim P1-F4A
 with sigma of 0.02
 P2-F7 \\sim P2-F8 \\sim P2-F9 \\sim P2-F10 \\sim P2-F11 \\sim P2-F12 \\sim
P2-F12A \\sim P2-F8A \\sim P2-F9A
 \\sim P2-F11A
 with sigma of 0.02
 F1-F2 \\sim F1-F3 \\sim F1-F4 \\sim F1-F5 \\sim F2-F3 \\sim F2-F5 \\sim F2-F6
\\sim F3-F4 \\sim F3-F6 \\sim F4-F5
 \\sim F4-F6 \\sim F5-F6 \\sim F6A-F5A \\sim F6A-F3A \\sim F6A-F2A \\sim
F6A-F4A \\sim F5A-F1A \\sim F5A-F2A ~
 F5A-F4A \\sim F1A-F3A \\sim F1A-F2A \\sim F1A-F4A \\sim F3A-F2A \\sim F3A-F4A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
F8A \\sim F8: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
F12 \\sim F12A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
F2A \\sim F2: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
F11 \\sim F11A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C5 \\sim C5A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
C6 \\sim C6A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
F9 \\sim F9A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
F4A \\sim F4: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
F5A \\sim F1: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
F6 \\sim F3A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
4. Rigid body (RIGU) restrains
 P2, F7, F8, F9, F10, F11, F12, F12A, F8A, F9A, F11A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 P1, F1, F2, F3, F4, F5, F6, F6A, F5A, F1A, F3A, F2A, F4A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N3, N4, C5, C5A, C6, C6A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=1-FVAR(1)
 Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(C6)=Sof(H6A)=Sof(H6B)=FVAR(1)
 Sof(F6A)=Sof(F5A)=Sof(F1A)=Sof(F3A)=Sof(F2A)=Sof(F4A)=1-FVAR(2)
 Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=FVAR(2)
 Sof(F12A)=Sof(F8A)=Sof(F9A)=Sof(F11A)=1-FVAR(3)
 Sof(F8)=Sof(F9)=Sof(F11)=Sof(F12)=FVAR(3)
6.a Ternary CH refined with riding coordinates:
 N1(H1), N2(H2), N3(H3), N4(H4), N5(H5)
6.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C5A(H5AA,
 H5AB), C6(H6A,H6B), C6A(H6AA,H6AB), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B),
 C10(H10A,H10B)
6.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              6136
_shelx_hkl_checksum              72263
_olex2_submission_special_instructions 'No special instructions were received'