Trapping of soluble, KCl-stabilized Cu(I) hydrides with CO<sub>2</sub> gives crystalline formates.
Grasruck, Alexander; Parla, Giorgio; Lou, Lisha; Langer, Jens; Neiß, Christian; Herrera, Alberto; Frieß, Sybille; Görling, Andreas; Schmid, Günter; Dorta, Romano; Chemical communications (Cambridge, England)  (2023) –; doi:10.1039/d3cc03033d

data_7132309
_publ_section_title
;
 Trapping of soluble, KCl-stabilized Cu(I) hydrides with CO<sub>2</sub>
 gives crystalline formates.
;
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_paper_doi               10.1039/d3cc03033d
_journal_year                    2023
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C40.891 H48.891 Cl0.109 Cu N2 O1.782 P2'
_chemical_formula_sum            'C40.89 H48.89 Cl0.11 Cu N2 O1.78 P2'
_chemical_formula_weight         726.29
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-04-11
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2023-05-24 deposited with the CCDC.	2023-10-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.29438(6)
_cell_length_b                   15.43040(8)
_cell_length_c                   23.74742(11)
_cell_measurement_reflns_used    23182
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      72.6770
_cell_measurement_theta_min      3.7010
_cell_volume                     3772.19(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -114.00 -13.00   1.00    1.00    --  -41.44 -57.00-150.00  101
  2  \w    -39.00  82.00   1.00    1.00    --   41.44 -19.00-180.00  121
  3  \w     32.00 133.00   1.00    3.30    --  104.37 -61.00   0.00  101
  4  \w     76.00 178.00   1.00    3.30    --  104.37  30.00 150.00  102
  5  \w     31.00 112.00   1.00    3.30    --  104.37-125.00 -30.00   81
  6  \w     31.00 112.00   1.00    3.30    --  104.37-125.00  60.00   81
  7  \w     97.00 178.00   1.00    3.30    --  104.37 125.00 -60.00   81
  8  \w   -114.00 -13.00   1.00    1.00    --  -41.44 -57.00 -30.00  101
  9  \w    -86.00  -6.00   1.00    1.00    --  -41.44 125.00   0.00   80
 10  \w     52.00 178.00   1.00    3.30    --  104.37  15.00 -60.00  126
 11  \w     75.00 177.00   1.00    3.30    --  104.37  61.00  90.00  102
 12  \w     75.00 116.00   1.00    3.30    --  104.37  61.00-180.00   41
 13  \w     79.00 177.00   1.00    3.30    --  104.37  45.00  30.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0009585000
_diffrn_orient_matrix_UB_12      -0.0971849000
_diffrn_orient_matrix_UB_13      -0.0149099000
_diffrn_orient_matrix_UB_21      0.0424653000
_diffrn_orient_matrix_UB_22      -0.0221153000
_diffrn_orient_matrix_UB_23      0.0605254000
_diffrn_orient_matrix_UB_31      -0.1434823000
_diffrn_orient_matrix_UB_32      -0.0058665000
_diffrn_orient_matrix_UB_33      0.0179831000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_unetI/netI     0.0275
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            28583
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.675
_diffrn_reflns_theta_min         3.416
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.963
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.543
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_description       block
_exptl_crystal_F_000             1533
_exptl_crystal_size_max          0.224
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.436
_refine_diff_density_min         -0.410
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details
;
 Flack x determined using 3134 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.010(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         7366
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0319
_refine_ls_R_factor_gt           0.0317
_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^)+(0.0566P)^2^+0.9931P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0827
_refine_ls_wR_factor_ref         0.0829
_reflns_Friedel_coverage         0.771
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.972
_reflns_number_gt                7302
_reflns_number_total             7366
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc03033d2.cif
_cod_data_source_block           rodo190905b
_cod_database_code               7132309
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C40.9H48.9Cl0.1CuN2O1.8P2
_shelx_estimated_absorpt_t_max   0.828
_shelx_estimated_absorpt_t_min   0.668
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(Cl1) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
3. Others
 Sof(Cl1)=1-FVAR(1)
 Sof(O1)=Sof(O2)=Sof(C1)=Sof(H1)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C16(H16), C19(H19), C36(H36), C39(H39)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C11(H11), C12(H12), C13(H13),
 C14(H14), C23(H23), C24(H24), C25(H25), C26(H26), C28(H28), C29(H29), C31(H31),
  C32(H32), C33(H33), C34(H34), C1(H1)
4.c Idealised Me refined as rotating group:
 C17(H17a,H17b,H17c), C18(H18a,H18b,H18c), C20(H20a,H20b,H20c), C21(H21a,H21b,
 H21c), C37(H37a,H37b,H37c), C38(H38a,H38b,H38c), C40(H40a,H40b,H40c), C41(H41a,
 H41b,H41c)
;
_shelx_res_checksum              84508
_shelx_hkl_checksum              72496
_olex2_date_sample_data_collection 2021-07-01
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.216
_oxdiff_exptl_absorpt_empirical_full_min 0.797