Exploring the effect of pressure on the crystal structure and caloric properties of the molecular ionic hybrid [(CH<sub>3</sub>)<sub>3</sub>NOH]<sub>2</sub>[CoCl<sub>4</sub>].
Dafonte-Rodríguez, Pedro; Delgado-Ferreiro, Ignacio; García-Ben, Javier; Ferradanes-Martínez, Angel; Gelpi, María; Walker, Julian; McMonagle, Charles James; Castro-García, Socorro; Señarís-Rodríguez, María Antonia; Bermúdez-García, Juan Manuel; Sánchez-Andújar, Manuel; Chemical communications (Cambridge, England) 60 (2024) 14065–14068; doi:10.1039/d4cc05125d

data_7133941
_publ_section_title
;
 Exploring the effect of pressure on the crystal structure and caloric
 properties of the molecular ionic hybrid
 [(CH<sub>3</sub>)<sub>3</sub>NOH]<sub>2</sub>[CoCl<sub>4</sub>].
;
_journal_issue                   95
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              14065
_journal_page_last               14068
_journal_paper_doi               10.1039/d4cc05125d
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'Cl4 Co, 2(C3 H10 N O)'
_chemical_formula_sum            'C6 H20 Cl4 Co N2 O2'
_chemical_formula_weight         352.97
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2024-03-08
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-09-26 deposited with the CCDC.	2024-11-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.772(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.4749(6)
_cell_length_b                   12.0762(8)
_cell_length_c                   15.0400(10)
_cell_measurement_reflns_used    5587
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      35.775
_cell_measurement_theta_min      2.757
_cell_volume                     1512.14(18)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON-III C14'
_diffrn_measurement_method       '\f or \w oscillation scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0488
_diffrn_reflns_av_unetI/netI     0.0258
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7342
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.341
_diffrn_reflns_theta_min         2.178
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.827
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0744 before and 0.0642 after correction.
 
For component 2:
 wR2(int) was 0.0977 before and 0.0713 after correction.
 The Ratio of minimum to maximum transmission is 0.89.

Final HKLF 4 output contains 121847 reflections, Rint = 0.0593
 (74302 with I > 3sig(I), Rint = 0.0545)
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_description       block
_exptl_crystal_F_000             724
_exptl_crystal_size_max          0.205
_exptl_crystal_size_mid          0.153
_exptl_crystal_size_min          0.152
_exptl_transmission_factor_max   0.758
_exptl_transmission_factor_min   0.722
_refine_diff_density_max         0.409
_refine_diff_density_min         -0.587
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     144
_refine_ls_number_reflns         7298
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0281
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0177P)^2^+0.6254P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0547
_refine_ls_wR_factor_ref         0.0572
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6382
_reflns_number_total             7342
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc05125d2.cif
_cod_data_source_block           23cgc013bt100k
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7133941--7133942.cif.
;
_cod_database_code               7133941
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.769
_shelx_estimated_absorpt_t_min   0.706
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C2(H2A,H2B,H2C), C1(H1A,
 H1B,H1C), C3(H3A,H3B,H3C)
2.b Idealised tetrahedral OH refined as rotating group:
 O2(H2), O1(H1)
;
_olex2_submission_special_instructions 'No special instructions were received'