Unravelling strong temperature-dependence of <i>J</i><sub>HD</sub> in transition metal hydrides: solvation and non-covalent interactions <i>versus</i> temperature-elastic H-H bonds.
Polukeev, Alexey V.; Capelli, Silvia C.; Wendt, Ola F.; Chemical science 14 (2023) 12308–12320; doi:10.1039/d3sc04197b

data_1570119
_publ_section_title
;
 Unravelling strong temperature-dependence of <i>J</i><sub>HD</sub> in
 transition metal hydrides: solvation and non-covalent interactions
 <i>versus</i> temperature-elastic H-H bonds.
;
_journal_issue                   43
_journal_name_full               'Chemical science'
_journal_page_first              12308
_journal_page_last               12320
_journal_paper_doi               10.1039/d3sc04197b
_journal_volume                  14
_journal_year                    2023
_chemical_formula_sum            'C22 H41 Ir O2 P2'
_chemical_formula_weight         591.69
_chemical_name_common            '[2,6-(tBu2PO)2-C6H3]IrH2'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2023-05-15 deposited with the CCDC.	2023-10-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.75(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.656(9)
_cell_length_b                   10.538(5)
_cell_length_c                   15.607(8)
_cell_measurement_reflns_used    550
_cell_measurement_temperature    10(2)
_cell_measurement_theta_max      84.322
_cell_measurement_theta_min      9.304
_cell_volume                     2488(2)
_computing_cell_refinement       'SXD2001 (Gutmann, 2005)'
_computing_data_collection       SECI
_computing_data_reduction        'SXD2001 (Gutmann, 2005)'
_computing_molecular_graphics    'Mercury 3.6, (CCDC 2015)'
_computing_publication_material  'Mercury 3.6, (CCDC 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      10(2)
_diffrn_detector                 'scintillation counters'
_diffrn_detector_area_resol_mean 0.33
_diffrn_detector_details
;
Array of eleven flat square fiber-otpically coupled scintillator PSD 
with 64 x 64 pixels and active area of 192 x 192 mm each
(resolution: 0.33 by 0.33 pixels/mm)
;
_diffrn_measured_fraction_theta_full 668700.000
_diffrn_measured_fraction_theta_max 668700.000
_diffrn_measurement_device_type  'time-of-flight diffractometer'
_diffrn_measurement_method       'time-of-flight profile data'
_diffrn_radiation_type           neutron
_diffrn_radiation_wavelength_id  white-beam
_diffrn_reflns_av_unetI/netI     0.1072
_diffrn_reflns_Laue_measured_fraction_full 668700.000
_diffrn_reflns_Laue_measured_fraction_max 668700.000
_diffrn_reflns_limit_h_max       53
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            12875
_diffrn_reflns_point_group_measured_fraction_full 668700.000
_diffrn_reflns_point_group_measured_fraction_max 668700.000
_diffrn_reflns_theta_full        NaN
_diffrn_reflns_theta_max         84.322
_diffrn_reflns_theta_min         9.304
_diffrn_source                   'spallation source'
_exptl_absorpt_coefficient_mu    0.036
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          5
_exptl_crystal_size_mid          3
_exptl_crystal_size_min          1
_refine_diff_density_max         3.178
_refine_diff_density_min         -3.440
_refine_diff_density_rms         0.568
_refine_ls_extinction_coef       0.00056(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     438
_refine_ls_number_reflns         12875
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0988
_refine_ls_R_factor_gt           0.0962
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2382
_refine_ls_wR_factor_ref         0.2426
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12522
_reflns_number_total             12875
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc04197b2.cif
_cod_data_source_block           irh2_10_li
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

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

 Adding full bibliography for 1570117--1570122.cif.
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1570119
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              16931