Novel dinuclear open <i>paddle-wheel-like</i> copper complexes involving π-stacking on the basis of chiral binaphthyl phosphoric acid {(<i>R</i>)-PhosH}: structural, magnetic and optical properties.
Rodríguez, Humberto A; Cruz, Daniel A.; Lavín, Víctor; Padrón, Juan I; Lorenzo-Luis, Pablo; Dalton transactions (Cambridge, England : 2003) 53 (2024) 18099–18103; doi:10.1039/d4dt02044h

data_7717239
_publ_section_title
;
 Novel dinuclear open <i>paddle-wheel-like</i> copper complexes involving
 &#x3c0;-stacking on the basis of chiral binaphthyl phosphoric acid
 {(<i>R</i>)-PhosH}: structural, magnetic and optical properties.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              18099
_journal_page_last               18103
_journal_paper_doi               10.1039/d4dt02044h
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety
'0.5(C86 H62 Cu2 O19 P4), 0.5(C83 H58 Cu2 O19 P4), C3 H6 O, 0.75[C3H6O]'
_chemical_formula_sum            'C175 H132 Cu4 O40 P8'
_chemical_formula_weight         3376.72
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-08-29
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-08-29 deposited with the CCDC.	2024-10-17 downloaded from the CCDC.
;
_cell_angle_alpha                107.266(2)
_cell_angle_beta                 101.455(2)
_cell_angle_gamma                105.492(2)
_cell_formula_units_Z            1
_cell_length_a                   11.2551(2)
_cell_length_b                   18.5480(3)
_cell_length_c                   22.4544(5)
_cell_measurement_reflns_used    40726
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      73.0410
_cell_measurement_theta_min      3.9640
_cell_volume                     4112.34(17)
_computing_cell_refinement       'CrysAlisPro 1.171.43.104a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 42.93a (release 05-06-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.104a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5953
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.982
_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     -4.00  21.00   1.00    1.00    --   34.00  91.00 -92.12   25
  2  \w     -4.00  23.00   1.00    1.00    --   34.00  92.00 145.58   27
  3  \w    -20.00  29.00   1.00    1.00    --  -41.48  38.00  90.00   49
  4  \w    -12.00  20.00   1.00    1.00    --  -41.48  38.00  60.00   32
  5  \w   -112.00 -17.00   1.00    1.00    --  -41.48 -38.00  90.00   95
  6  \w     -3.00  36.00   1.00    1.00    --  -41.48  19.00  30.00   39
  7  \w   -113.00 -17.00   1.00    1.00    --  -41.48 -38.00 -90.00   96
  8  \w   -107.00 -17.00   1.00    1.00    --  -41.48 -38.00   0.00   90
  9  \w     27.00  95.00   1.00    1.00    --   41.48-125.00   0.00   68
 10  \w     29.00  96.00   1.00    1.00    --   41.48-125.00 150.00   67
 11  \w     16.00  42.00   1.00    1.00    --   50.00  81.00 171.34   26
 12  \w     16.00  42.00   1.00    1.00    --   50.00  82.00-110.04   26
 13  \w     16.00  41.00   1.00    1.00    --   50.00  82.00 -38.93   25
 14  \w     16.00  42.00   1.00    1.00    --   50.00  82.00  36.15   26
 15  \w     16.00  42.00   1.00    1.00    --   50.00  81.00  99.83   26
 16  \w     31.00  58.00   1.00    1.00    --   62.00  71.00   0.99   27
 17  \w     39.00  66.00   1.00    1.00    --   70.00  71.00  65.52   27
 18  \w    114.00 141.00   1.00    1.00    --   70.00  69.00 -80.40   27
 19  \w     39.00  66.00   1.00    1.00    --   70.00  69.00-119.40   27
 20  \w     39.00  75.00   1.00    1.00    --   70.00  69.00 -80.40   36
 21  \w     39.00  65.00   1.00    1.00    --   70.00  70.00 160.83   26
 22  \w     39.00  66.00   1.00    1.00    --   70.00  69.00 134.21   27
 23  \w    112.00 139.00   1.00    1.00    --   70.00  70.00 103.90   27
 24  \w     39.00  69.00   1.00    1.00    --   70.00  70.00-162.01   30
 25  \w     40.00  66.00   1.00    1.00    --   70.00  70.00 103.90   26
 26  \w     39.00  64.00   1.00    1.00    --   70.00  71.00  23.52   25
 27  \w    115.00 141.00   1.00    1.00    --   70.00  71.00  65.52   26
 28  \w    106.00 145.00   1.00    5.00    --   74.00  69.00 -34.08   39
 29  \w     43.00  78.00   1.00    5.00    --   74.00  69.00 -34.08   35
 30  \w     52.00  87.00   1.00    5.00    --   82.00  67.00  12.18   35
 31  \w    116.00 155.00   1.00    5.00    --   82.00  67.00  12.18   39
 32  \w     77.00 104.00   1.00    5.00    --  105.95  61.00 -30.00   27
 33  \w     77.00 105.00   1.00    5.00    --  105.95  61.00 -60.00   28
 34  \w     34.00  93.00   1.00    5.00    --  105.95 -61.00-150.00   59
 35  \w     84.00 111.00   1.00    5.00    --  105.95-125.00-150.00   27
 36  \w     37.00 112.00   1.00    5.00    --  105.95-125.00  60.00   75
 37  \w    117.00 173.00   1.00    5.00    --  105.95  61.00  60.00   56
 38  \w     77.00 110.00   1.00    5.00    --  105.95  61.00  60.00   33
 39  \w     35.00  93.00   1.00    5.00    --  105.95 -61.00  90.00   58
 40  \w     77.00 104.00   1.00    5.00    --  105.95  61.00  90.00   27
 41  \w    126.00 152.00   1.00    5.00    --  105.95  61.00-150.00   26
 42  \w    113.00 177.00   1.00    5.00    --  105.95  61.00-180.00   64
 43  \w     77.00 117.00   1.00    5.00    --  105.95  61.00-150.00   40
 44  \w    107.00 178.00   1.00    5.00    --  105.95  61.00 120.00   71
 45  \w     77.00 104.00   1.00    5.00    --  105.95  61.00-180.00   27
 46  \w     77.00 105.00   1.00    5.00    --  105.95  61.00 120.00   28
 47  \w     77.00 169.00   1.00    5.00    --  105.95  61.00-120.00   92
 48  \w    117.00 175.00   1.00    5.00    --  105.95  61.00  30.00   58
 49  \w    119.00 153.00   1.00    5.00    --  105.95  61.00  90.00   34
 50  \w     77.00 104.00   1.00    5.00    --  105.95  61.00  30.00   27
 51  \w     56.00 109.00   1.00    5.00    --  105.95-125.00   0.00   53
 52  \w    102.00 127.00   1.00    5.00    --  105.95 -77.00 -60.00   25
 53  \w     77.00 103.00   1.00    5.00    --  105.95  61.00   0.00   26
 54  \w    111.00 168.00   1.00    5.00    --  105.95  61.00   0.00   57
 55  \w    111.00 170.00   1.00    5.00    --  105.95  61.00 -90.00   59
 56  \w     30.00  85.00   1.00    5.00    --  105.95 -77.00 -60.00   55
 57  \w     77.00 104.00   1.00    5.00    --  105.95  61.00 -90.00   27
 58  \w     27.00 106.00   1.00    5.00    --  105.95 -95.00-153.06   79
 59  \w    113.00 152.00   1.00    5.00    --  105.95  61.00 150.00   39
 60  \w    108.00 170.00   1.00    5.00    --  105.95  61.00 -60.00   62
 61  \w     25.00 107.00   1.00    5.00    --  105.95 -97.00  88.87   82
 62  \w     77.00 106.00   1.00    5.00    --  105.95  61.00 150.00   29
 63  \w    111.00 155.00   1.00    5.00    --  105.95  61.00 -30.00   44
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0092955000
_diffrn_orient_matrix_UB_12      -0.0867468000
_diffrn_orient_matrix_UB_13      -0.0370858000
_diffrn_orient_matrix_UB_21      0.1470511000
_diffrn_orient_matrix_UB_22      0.0238535000
_diffrn_orient_matrix_UB_23      0.0295174000
_diffrn_orient_matrix_UB_31      -0.0220985000
_diffrn_orient_matrix_UB_32      -0.0227143000
_diffrn_orient_matrix_UB_33      0.0585921000
_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  0.0326
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            67768
_diffrn_reflns_point_group_measured_fraction_full 0.951
_diffrn_reflns_point_group_measured_fraction_max 0.921
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.165
_diffrn_reflns_theta_min         4.004
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.967
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.552
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.104a (Rigaku Oxford Diffraction, 2023)
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            'light blue'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1738
_exptl_crystal_size_max          0.215
_exptl_crystal_size_mid          0.195
_exptl_crystal_size_min          0.158
_refine_diff_density_max         0.787
_refine_diff_density_min         -0.709
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details
;
 Flack x determined using 12155 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.004(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2107
_refine_ls_number_reflns         30348
_refine_ls_number_restraints     197
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0507
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1058P)^2^+1.8981P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1526
_refine_ls_wR_factor_ref         0.1580
_reflns_Friedel_coverage         0.877
_reflns_Friedel_fraction_full    0.904
_reflns_Friedel_fraction_max     0.861
_reflns_number_gt                28335
_reflns_number_total             30348
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02044h2.cif
_cod_data_source_block           hbr84b_01
_cod_depositor_comments          'Adding full bibliography for 7717239.cif.'
_cod_original_cell_volume        4112.34(15)
_cod_database_code               7717239
_shelx_shelxl_version_number     2019/3
_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, All O(H,H) groups
2. Restrained distances
 C63C-O61C \\sim C62C-O61C
 with sigma of 0.04
 C42C-O41C \\sim C43C-O41C
 with sigma of 0.04
 C33C-O31C \\sim C32C-O31C
 with sigma of 0.04
 C52C-O51C \\sim C53C-O51C
 with sigma of 0.04
3. Restrained planarity
 O61C, C61C, C63C, C62C
 with sigma of 0.05
 O41C, C41C, C42C, C43C
 with sigma of 0.05
 O51C, C51C, C52C, C53C
 with sigma of 0.05
 O31C, C31C, C33C, C32C
 with sigma of 0.05
4. Uiso/Uaniso restraints and constraints
O31C \\sim C31C \\sim C33C \\sim C32C: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
O41C \\sim C41C \\sim C42C \\sim C43C: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
O51C \\sim C51C \\sim C52C \\sim C53C: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
O61C \\sim C61C \\sim C63C \\sim C62C: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
C31A \\sim O3A \\sim C32A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C23A \\sim C21A \\sim C22A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C21A \\sim C23A \\sim C22A: within 2A with sigma of 0.002 and sigma for
terminal atoms of 0.004 within 2A
C32A \\sim C31A \\sim C33A: within 2A with sigma of 0.002 and sigma for
terminal atoms of 0.004 within 2A
C43A \\sim C41A \\sim C42A: within 2A with sigma of 0.002 and sigma for
terminal atoms of 0.004 within 2A
5. Rigid body (RIGU) restrains
 O41C, C41C, C42C, C43C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O31C, C31C, C33C, C32C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O61C, C61C, C63C, C62C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O51C, C51C, C52C, C53C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C61C, O61C, C63C, C62C, H63A, H63B, H63C, H62A, H62B, H62C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C51C, O51C, C52C, C53C, H52A, H52B, H52C, H53A, H53B, H53C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: O51C(0.5) C51C(0.5) C52C(0.5) H52A(0.5) H52B(0.5) H52C(0.5)
 C53C(0.5) H53A(0.5) H53B(0.5) H53C(0.5) O41C(0.5) C41C(0.5) C42C(0.5)
 H42D(0.5) H42E(0.5) H42F(0.5) C43C(0.5) H43D(0.5) H43E(0.5) H43F(0.5)
 O61C(0.5) C61C(0.5) C63C(0.5) H63A(0.5) H63B(0.5) H63C(0.5) C62C(0.5)
 H62A(0.5) H62B(0.5) H62C(0.5) O31C(0.5) C31C(0.5) C33C(0.5) H33D(0.5)
 H33E(0.5) H33F(0.5) C32C(0.5) H32D(0.5) H32E(0.5) H32F(0.5)
7.a Free rotating group:
 O51C(C51C,C52C,C53C), O41C(C41C,C42C,C43C), O61C(C61C,C63C,C62C), O31C(C31C,
 C33C,C32C)
7.b Rotating group:
 O2W(H2WA,H2WB), O4W(H4WA,H4WB), O1W(H1WA,H1WB)
7.c Me refined with riding coordinates:
 C32A(H32A,H32B,H32C), C63C(H63A,H63B,H63C)
7.d Aromatic/amide H refined with riding coordinates:
 C19G(H19G), C13A(H13A), C19A(H19A), C2G(H2G), C18G(H18G), C18A(H18A),
 C2H(H2H), C2C(H2C), C2F(H2F), C16A(H16A), C13B(H13B), C18F(H18F), C19C(H19C),
 C19F(H19F), C3D(H3D), C2D(H2D), C2A(H2A), C2E(H2E), C7C(H7C), C3A(H3A),
 C13G(H13G), C19D(H19D), C18C(H18C), C8C(H8C), C18E(H18E), C3F(H3F), C8D(H8D),
 C18D(H18D), C13E(H13E), C19E(H19E), C19B(H19B), C15A(H15A), C3H(H3H),
 C13F(H13F), C3B(H3B), C14E(H14E), C16G(H16G), C8E(H8E), C7D(H7D), C13H(H13H),
 C14A(H14A), C14F(H14F), C13C(H13C), C3C(H3C), C16F(H16F), C5D(H5D), C7B(H7B),
 C18B(H18B), C16D(H16D), C16E(H16E), C6C(H6C), C14D(H14D), C6B(H6B), C2B(H2B),
 C15E(H15E), C15F(H15F), C8H(H8H), C5B(H5B), C5A(H5A), C3E(H3E), C5G(H5G),
 C3G(H3G), C5C(H5C), C8F(H8F), C8B(H8B), C18H(H18H), C14G(H14G), C16B(H16B),
 C6G(H6G), C13D(H13D), C16C(H16C), C14C(H14C), C8A(H8A), C7H(H7H), C7E(H7E),
 C8G(H8G), C6A(H6A), C14B(H14B), C5H(H5H), C16H(H16H), C7G(H7G), C5F(H5F),
 C15C(H15C), C15G(H15G), C5E(H5E), C7F(H7F), C15D(H15D), C14H(H14H), C6E(H6E),
 C6H(H6H), C19H(H19H), C7A(H7A), C15B(H15B), C6D(H6D), C15H(H15H), C6F(H6F)
7.e Idealised Me refined as rotating group:
 C42A(H42A,H42B,H42C), C22A(H22A,H22B,H22C), C52C(H52A,H52B,H52C), C53C(H53A,
 H53B,H53C), C42C(H42D,H42E,H42F), C43C(H43D,H43E,H43F), C62C(H62A,H62B,H62C),
 C33C(H33D,H33E,H33F), C32C(H32D,H32E,H32F), C33A(H33A,H33B,H33C), C23A(H23A,
 H23B,H23C), C43A(H43A,H43B,H43C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 49 electrons were
found in a volume of 185\%A^3^ in 2 voids per unit cell.
This is consistent with the presence of
0.75[C3H6O] per formula unit
which account for 48 electrons
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              39837
_shelx_hkl_checksum              7370
_shelx_fab_checksum              66543
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.177
_oxdiff_exptl_absorpt_empirical_full_min 0.882