Reactivity among first and second coordination spheres using a multiprotonated ligand and Cu(ii) in the solid-state
Li, Haitao; Yang, Yuxia; Famulari, Antonino; Xin, Lianxin; Martí-Rujas, Javier; Guo, Fang; CrystEngComm 21 (2019) 4354–; doi:10.1039/C9CE00783K

data_7234919
_publ_section_title
;
 Reactivity among first and second coordination spheres using a
 multiprotonated ligand and Cu(ii) in the solid-state
;
_journal_issue                   29
_journal_name_full               CrystEngComm
_journal_page_first              4354
_journal_paper_doi               10.1039/C9CE00783K
_journal_volume                  21
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_moiety         'Cl4 Cu, 2(Cl), C18 H28 N4'
_chemical_formula_sum            'C18 H28 Cl6 Cu N4'
_chemical_formula_weight         576.68
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-06-12
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-06-12 deposited with the CCDC.	2019-06-19 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.7107(8)
_cell_length_b                   23.0021(14)
_cell_length_c                   7.9717(4)
_cell_measurement_reflns_used    6595
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.20
_cell_measurement_theta_min      2.31
_cell_volume                     2514.1(2)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      149.65
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_unetI/netI     0.0593
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            11177
_diffrn_reflns_theta_full        25.07
_diffrn_reflns_theta_max         25.07
_diffrn_reflns_theta_min         2.97
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.520
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6972
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0929 before and 0.0628 after correction.
The Ratio of minimum to maximum transmission is 0.9356.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1180
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.939
_refine_diff_density_min         -0.962
_refine_diff_density_rms         0.104
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         4428
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0864
_refine_ls_R_factor_gt           0.0646
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0797P)^2^+7.0874P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1546
_refine_ls_wR_factor_ref         0.1669
_reflns_number_gt                3553
_reflns_number_total             4428
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c9ce00783k2.cif
_cod_data_source_block           gf01_a
_cod_database_code               7234919
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
2. Uiso/Uaniso restraints and constraints
C18 \\sim C17 \\sim C16: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.01
N4 \\sim C6 \\sim C7: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.01
Uanis(N3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Sof(Cl4')=1-FVAR(1)
 Sof(Cl4)=FVAR(1)
 Sof(Cl1')=1-FVAR(2)
 Sof(Cl1)=FVAR(2)
 Fixed Sof: Cl5(0.5)
4.a Ternary CH refined with riding coordinates:
 C2(H2), C1(H1)
4.b Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B), C3(H3A,H3B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,
 H11B), C12(H12A,H12B), C13(H13A,H13B)
4.c Aromatic/amide H refined with riding coordinates:
 N4(H4), N3(H3), C5(H5), C6(H6), C7(H7), C8(H8), C18(H18), C17(H17), C16(H16),
 C15(H15)
;
_olex2_submission_special_instructions 'No special instructions were received'