Zero area thermal expansion of honeycomb layers via double distortion relaxation in (PPh4)[Cu2(CN)3]
Iwai, Yudai; Nakaya, Manabu; Ohtsu, Hiroyoshi; Le Ouay, Benjamin; Ohtani, Ryo; Ohba, Masaaki; CrystEngComm  (2022) –; doi:10.1039/D2CE00878E

data_7245217
_publ_section_title
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 Zero area thermal expansion of honeycomb layers via double distortion
 relaxation in (PPh4)[Cu2(CN)3]
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00878E
_journal_year                    2022
_chemical_formula_moiety         'C3 H3 Cu2 N3, 0.5(C48 H40 P2)'
_chemical_formula_sum            'C27 H23 Cu2 N3 P'
_chemical_formula_weight         544.545
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_Int_Tables_number      62
_audit_creation_date             2022-04-25
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2022.04.21 svn.rca3783a0 for OlexSys, GUI svn.r6444)
;
_audit_update_record
;
2022-06-27 deposited with the CCDC.	2022-07-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.3204(9)
_cell_length_b                   18.8505(13)
_cell_length_c                   8.9253(6)
_cell_measurement_reflns_used    2609
_cell_measurement_temperature    200.0
_cell_measurement_theta_max      23.14
_cell_measurement_theta_min      2.52
_cell_volume                     2409.4(3)
_computing_data_collection       'APEX3 (Bruker AXS, 2019)'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-dev (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      196.00
_diffrn_measured_fraction_theta_full 0.9978
_diffrn_measured_fraction_theta_max 0.9978
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0846
_diffrn_reflns_av_unetI/netI     0.0447
_diffrn_reflns_Laue_measured_fraction_full 0.9978
_diffrn_reflns_Laue_measured_fraction_max 0.9978
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            17409
_diffrn_reflns_point_group_measured_fraction_full 0.9978
_diffrn_reflns_point_group_measured_fraction_max 0.9978
_diffrn_reflns_theta_full        23.4943
_diffrn_reflns_theta_max         23.49
_diffrn_reflns_theta_min         2.52
_exptl_absorpt_coefficient_mu    1.851
_exptl_absorpt_correction_T_max  0.7449
_exptl_absorpt_correction_T_min  0.6164
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1043 before and 0.0732 after correction.
The Ratio of minimum to maximum transmission is 0.8275.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_description       block
_exptl_crystal_F_000             1107.826
_exptl_crystal_size_max          0.158
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.067
_refine_diff_density_max         0.4620
_refine_diff_density_min         -0.5495
_refine_diff_density_rms         0.1063
_refine_ls_d_res_high            0.8914
_refine_ls_d_res_low             8.0668
_refine_ls_goodness_of_fit_ref   1.0581
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    54
_refine_ls_number_parameters     206
_refine_ls_number_reflns         1834
_refine_ls_number_restraints     198
_refine_ls_restrained_S_all      0.9991
_refine_ls_R_factor_all          0.0695
_refine_ls_R_factor_gt           0.0426
_refine_ls_shift/su_max          0.0007
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0535P)^2^+2.8620P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1067
_refine_ls_wR_factor_ref         0.1233
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              16
_reflns_limit_h_min              0
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              9
_reflns_limit_l_min              0
_reflns_number_gt                1305
_reflns_number_total             1834
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2ce00878e2.cif
_cod_data_source_block           pph4cu_200K
_cod_database_code               7245217
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H,H) groups
2. Shared sites
{N005, C1}
{C007, N1}
{N0, C008}
3. Uiso/Uaniso restraints and constraints
Uanis(N0) = Uanis(C008)
Uanis(N005) = Uanis(C1)
Uanis(C008) = Uanis(N0)
Uanis(C007) = Uanis(N1)
4. Rigid body (RIGU) restrains
 P002, C003, C004, C006, C2, C00B, C3, C00A, C00F, C00C, C6, C4, C5, C00I, C7,
 C00H, C00J, C00E, C10, C8, C9, C009, C00G, C00D, C11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: N005(0.5) C007(0.5) C008(0.5) N0(0.5) N1(0.5) C1(0.5) C004(0.5)
 C2(0.5) C00B(0.5) C3(0.5) C00A(0.5) C00F(0.5) C00C(0.5) C6(0.5) C4(0.5)
 C5(0.5) C00I(0.5) C7(0.5) C00H(0.5) C00J(0.5) C00E(0.5) C10(0.5) C8(0.5)
 C9(0.5) C009(0.5) C00G(0.5) C00D(0.5) C11(0.5) H3(0.5) H7(0.5) H009(0.5)
 H00I(0.5) H00B(0.5) H00F(0.5) H00J(0.5) H00G(0.5) H00H(0.5) H00A(0.5) H6(0.5)
 H10(0.5) H00D(0.5) H00E(0.5) H00C(0.5) H5(0.5) H9(0.5) H11(0.5) H8(0.5)
 H4(0.5) H00k(0.5) H00l(0.5) H00m(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7), C009(H009), C00I(H00I), C00B(H00B), C00F(H00F), C00J(H00J),
 C00G(H00G), C00H(H00H), C00A(H00A), C6(H6), C10(H10), C00D(H00D), C00E(H00E),
 C00C(H00C), C5(H5), C9(H9), C11(H11), C8(H8), C4(H4)
6.b Fitted hexagon refined as free rotating group:
 C004(C00A,C00H,C00G,C00J,C00F), C006(C00C,C00E,C00D,C10,C6), C2(C4,C8,C11,C9,
 C5), C003(C00B,C00I,C009,C7,C3)
6.c Idealised Me refined as rotating group:
 N0(H00k,H00l,H00m)
;
_olex2_submission_special_instructions 'No special instructions were received'