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_7244211
_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 H21 Cl N5 Ru, F6 P'
_chemical_formula_sum            'C10 H21 Cl F6 N5 P Ru'
_chemical_formula_weight         492.81
_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                75.896(2)
_cell_angle_beta                 88.525(2)
_cell_angle_gamma                85.227(2)
_cell_formula_units_Z            2
_cell_length_a                   7.7456(7)
_cell_length_b                   10.3834(9)
_cell_length_c                   11.0010(10)
_cell_measurement_reflns_used    8664
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      31.149
_cell_measurement_theta_min      2.8775
_cell_volume                     855.10(13)
_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      150.0
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_Laue_measured_fraction_full 0.999
_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       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11091
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         31.149
_diffrn_reflns_theta_min         2.081
_diffrn_source                   'Advanced Light Source, station 11.3.1'
_exptl_absorpt_coefficient_mu    1.538
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6736
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2014.5 (Sheldrick)'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.914
_exptl_crystal_description       plate
_exptl_crystal_F_000             492
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.015
_refine_diff_density_max         0.502
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         4249
_refine_ls_number_restraints     331
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0258
_refine_ls_R_factor_gt           0.0235
_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^)+(0.0267P)^2^+0.4969P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0604
_refine_ls_wR_factor_ref         0.0618
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3973
_reflns_number_total             4249
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01534f2.cif
_cod_data_source_block           mg07bp1
_cod_depositor_comments
'Adding full bibliography for 7244202--7244217.cif.'
_cod_database_code               7244211
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.977
_shelx_estimated_absorpt_t_min   0.941
_olex2_refinement_description
;
1. Restrained distances
 P1-F2 \\sim P1-F2A
 with sigma of 0.02
 F2-F3 \\sim F2-F6 \\sim F3-F5 \\sim F5-F6 \\sim F6A-F2A \\sim F6A-F5A \\sim
F2A-F3A \\sim F3A-F5A
 with sigma of 0.04
 P1-F3 \\sim P1-F3A
 with sigma of 0.02
 P1-F5 \\sim P1-F5A
 with sigma of 0.02
 P1-F1 \\sim P1-F2 \\sim P1-F3 \\sim P1-F4 \\sim P1-F5 \\sim P1-F6 \\sim P1-F6A
\\sim P1-F2A \\sim P1-F3A \\sim P1-
 F5A
 with sigma of 0.02
 P1-F6 \\sim P1-F6A
 with sigma of 0.02
 N5-H5 \\sim N4-H4 \\sim N1-H1
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
P1 \\sim F1 \\sim F2 \\sim F2A \\sim F3 \\sim F3A \\sim F4 \\sim F5 \\sim F5A
\\sim F6 \\sim F6A: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08 within 2A
Uanis(F6A) \\sim Ueq, Uanis(F5A) \\sim Ueq, Uanis(F3A) \\sim Ueq, Uanis(F2A)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
3. Rigid body (RIGU) restrains
 P1, F1, F2, F2A, F3, F3A, F4, F5, F5A, F6, F6A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(F2A)=Sof(F3A)=Sof(F5A)=Sof(F6A)=1-FVAR(1)
 Sof(F2)=Sof(F3)=Sof(F5)=Sof(F6)=FVAR(1)
5.a Ternary CH refined with riding coordinates and stretchable bonds:
 N1(H1), N4(H4), N5(H5)
5.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B),
 C9(H9A,H9B), C10(H10A,H10B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4A)
;
_shelx_res_checksum              70551
_shelx_hkl_checksum              19704
_olex2_submission_special_instructions 'No special instructions were received'