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_7244215
_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         'C13.76 H30.64 Fe I0.12 N5 O3.76, F6 P'
_chemical_formula_sum            'C13.76 H30.64 F6 Fe I0.12 N5 O3.76 P'
_chemical_formula_weight         542.40
_space_group_crystal_system      orthorhombic
_space_group_IT_number           64
_space_group_name_Hall           '-C 2ac 2'
_space_group_name_H-M_alt        'C m c e'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.9648(14)
_cell_length_b                   19.2765(14)
_cell_length_c                   12.8235(10)
_cell_measurement_reflns_used    9932
_cell_measurement_temperature    150
_cell_measurement_theta_max      31.1725
_cell_measurement_theta_min      2.418
_cell_volume                     4440.8(6)
_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(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0429
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            28456
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         31.175
_diffrn_reflns_theta_min         2.304
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    1.253
_exptl_absorpt_correction_T_max  0.9281
_exptl_absorpt_correction_T_min  0.7985
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2014.5 (Sheldrick)'
_exptl_crystal_colour            'brownish orange'
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.623
_exptl_crystal_description       block
_exptl_crystal_F_000             2237
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.923
_refine_diff_density_min         -0.554
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         2871
_refine_ls_number_restraints     219
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0528
_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^)+(0.0946P)^2^+9.1471P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1538
_refine_ls_wR_factor_ref         0.1651
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2293
_reflns_number_total             2871
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01534f2.cif
_cod_data_source_block           dd07acmca
_cod_depositor_comments
'Adding full bibliography for 7244202--7244217.cif.'
_cod_original_sg_symbol_Hall     '-C 2bc 2'
_cod_database_code               7244215
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.963
_shelx_estimated_absorpt_t_min   0.917
_olex2_refinement_description
;
1. Restrained distances
 C6-H6B = C6-H6A
 0.99 with sigma of 0.02
 H6B-H6A
 1.62 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim
Ueq, Uanis(F4) \\sim Ueq, Uanis(O2A) \\sim Ueq, Uanis(O2B) \\sim Ueq: with
sigma of 0.004 and sigma for terminal atoms of 0.008
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: I1(0.06) O1(0.94) O2A(0.58) O2B(0.36) N3(0.5) H3(0.5) C4(0.5)
 H4A(0.5) H4B(0.5) C5(0.5) H5A(0.5) H5B(0.5) C6(0.5) C7(0.5) H7A(0.5) H7B(0.5)
 C8(0.94) C9(0.94) H9A(0.94) H9B(0.94) H9C(0.94) F1(0.5) F3(0.5) H6A(0.5)
 H6B(0.5)
 Fixed X: H3(0.287649)
 Fixed Y: H3(0.49303)
 Fixed Z: H3(0.155781)
5.a Ternary CH refined with riding coordinates:
 N2(H2)
5.b Ternary CH refined with riding coordinates and stretchable bonds:
 N1(H1)
5.c Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C7(H7A,H7B)
5.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C)
;
_shelx_res_checksum              46565
_shelx_hkl_checksum              6067
_olex2_submission_special_instructions 'No special instructions were received'