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_7244206
_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 Cl2 Fe N5'
_chemical_formula_sum            'C10 H25 Cl2 Fe N5'
_chemical_formula_weight         342.10
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_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                 100.133(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.9184(6)
_cell_length_b                   6.7907(5)
_cell_length_c                   14.7266(11)
_cell_measurement_reflns_used    9975
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      31.159
_cell_measurement_theta_min      4.4315
_cell_volume                     779.52(10)
_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)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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  0.0378
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15568
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         31.135
_diffrn_reflns_theta_min         2.988
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    1.642
_exptl_absorpt_correction_T_max  0.9281
_exptl_absorpt_correction_T_min  0.8105
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2014.5 (Sheldrick)'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_description       block
_exptl_crystal_F_000             360
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.452
_refine_diff_density_min         -0.302
_refine_diff_density_rms         0.040
_refine_ls_extinction_coef       0.0036(10)
_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   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         1936
_refine_ls_number_restraints     274
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.0231
_refine_ls_R_factor_gt           0.0203
_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^)+(0.0236P)^2^+0.2149P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0515
_refine_ls_wR_factor_ref         0.0529
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1780
_reflns_number_total             1936
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01534f2.cif
_cod_data_source_block           alb04
_cod_depositor_comments
'Adding full bibliography for 7244202--7244217.cif.'
_cod_database_code               7244206
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.968
_shelx_estimated_absorpt_t_min   0.937
_olex2_refinement_description
;
1. Restrained distances
 N1-H1 \\sim N2-H2 \\sim N4-H4 \\sim N5-H5 \\sim N3-H3
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.1 and sigma
for terminal atoms of 0.2
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: N1(0.5) H1(0.5) N3(0.5) H3(0.5) N2(0.5) H2(0.5) N4(0.5) H4(0.5)
 N5(0.5) H5(0.5) C1(0.5) H1A(0.5) H1B(0.5) C6(0.5) H6A(0.5) H6B(0.5) C2(0.5)
 H2A(0.5) H2B(0.5) C7(0.5) H7A(0.5) H7B(0.5) C3(0.5) H3A(0.5) H3B(0.5) C8(0.5)
 H8A(0.5) H8B(0.5) C4(0.5) H4A(0.5) H4B(0.5) C9(0.5) H9A(0.5) H9B(0.5) C5(0.5)
 H5A(0.5) H5B(0.5) C10(0.5) H10A(0.5) H10B(0.5)
5.a Ternary CH refined with riding coordinates and stretchable bonds:
 N1(H1), N3(H3), N2(H2), N4(H4), N5(H5)
5.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C6(H6A,H6B), C2(H2A,H2B), C7(H7A,H7B), C3(H3A,H3B), C8(H8A,H8B),
 C4(H4A,H4B), C9(H9A,H9B), C5(H5A,H5B), C10(H10A,H10B)
;
_shelx_res_checksum              25207
_shelx_hkl_checksum              49958
_olex2_submission_special_instructions 'No special instructions were received'