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_7244217
_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 Cl Co N5, Cl'
_chemical_formula_sum            'C10 H25 Cl2 Co N5'
_chemical_formula_weight         345.18
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_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            16
_cell_length_a                   14.5128(14)
_cell_length_b                   12.7676(11)
_cell_length_c                   32.102(3)
_cell_measurement_reflns_used    9944
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.9155
_cell_measurement_theta_min      2.767
_cell_volume                     5948.3(9)
_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
_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  0.1321
_diffrn_reflns_av_unetI/netI     0.0489
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            98328
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        27.646
_diffrn_reflns_theta_max         27.646
_diffrn_reflns_theta_min         2.063
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    1.898
_exptl_absorpt_correction_T_max  0.9037
_exptl_absorpt_correction_T_min  0.8703
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS v2014.5 (Sheldrick)'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_description       block
_exptl_crystal_F_000             2896
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.727
_refine_diff_density_min         -0.493
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         5348
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0742
_refine_ls_R_factor_gt           0.0416
_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^)+(0.0350P)^2^+9.1459P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0836
_refine_ls_wR_factor_ref         0.0958
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3774
_reflns_number_total             5348
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01534f2.cif
_cod_data_source_block           dsb04c-pbca
_cod_depositor_comments
'Adding full bibliography for 7244202--7244217.cif.'
_cod_original_cell_volume        5948.2(10)
_cod_database_code               7244217
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.945
_shelx_estimated_absorpt_t_min   0.911
_olex2_refinement_description
;
1. Restrained distances
 N9A-C17 \\sim N9A-C17A
 with sigma of 0.02
 N10-C20 \\sim N10-C20A
 with sigma of 0.04
 N9A-C18 \\sim N9A-C18A
 with sigma of 0.04
 N6-C20 \\sim N6-C20A
 with sigma of 0.02
 N9A-C17 \\sim N9-C17
 with sigma of 0.02
 N9A-C17A \\sim N9-C17A
 with sigma of 0.02
 Co2-N9A \\sim Co2-N9
 with sigma of 0.02
 N10-C19 \\sim N10-C19A
 with sigma of 0.02
 N9A-C16 \\sim N9-C16
 with sigma of 0.02
 C19-C20 \\sim C19A-C20A
 with sigma of 0.02
 C17-C18 \\sim C17A-C18A
 with sigma of 0.02
 N10-C17 \\sim N10-C17A
 with sigma of 0.04
 N6-C19 \\sim N6-C19A
 with sigma of 0.04
 N10-C18 \\sim N10-C18A
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
N9A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(N9A) = Uanis(N9)
Uanis(C17) = Uanis(C17A)
Uanis(C20A) = Uanis(C20)
Uanis(C19) = Uanis(C19A)
Uanis(C18A) = Uanis(C18)
3. Rigid body (RIGU) restrains
 N6, C20A, C20, C19A, C19, N10, C18A, C17A, C17, N9A, N9, C16
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(N9A)=Sof(H9A)=Sof(C20A)=Sof(H20C)=Sof(H20D)=Sof(C19A)=Sof(H19C)=Sof(H19D)=
 Sof(C18A)=Sof(H18C)=Sof(H18D)=Sof(C17A)=Sof(H17C)=Sof(H17D)=1-FVAR(1)
 Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(C19)=Sof(H19A)=
 Sof(H19B)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(N9)=Sof(H9)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 N1(H1), N2(H2), N3(H3), N4(H4), N5(H5), N6(H6), N7(H7), N8(H8), N9A(H9A),
 N10(H10), N9(H9)
5.b 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(H9B,H9C), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C17(H17A,H17B), C18(H18A,H18B),
  C19(H19A,H19B), C20(H20A,H20B), C20A(H20C,H20D), C19A(H19C,H19D), C18A(H18C,
 H18D), C17A(H17C,H17D)
;
_shelx_res_checksum              39788
_shelx_hkl_checksum              703
_olex2_submission_special_instructions 'No special instructions were received'