Macrocyclic bis-diphosphenes demonstrating bimetallic <i>exo</i>- and <i>endo</i>-cyclic binding modes.
Kreimer, Lisa N.; Hadlington, Terrance J.; Chemical science 15 (2024) 14154–14160; doi:10.1039/d4sc03516j

data_1572146
_publ_section_title
;
 Macrocyclic bis-diphosphenes demonstrating bimetallic <i>exo</i>- and
 <i>endo</i>-cyclic binding modes.
;
_journal_issue                   35
_journal_name_full               'Chemical science'
_journal_page_first              14154
_journal_page_last               14160
_journal_paper_doi               10.1039/d4sc03516j
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C22.50 H34 N2 Ni0.50 O P'
_chemical_formula_sum            'C22.5 H34 N2 Ni0.5 O P'
_chemical_formula_weight         408.84
_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   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-05-23 deposited with the CCDC.	2024-07-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.35(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.304(3)
_cell_length_b                   34.054(7)
_cell_length_c                   9.7484(19)
_cell_measurement_reflns_used    2000
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.50
_cell_measurement_theta_min      1.92
_cell_volume                     5038.8(18)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'STOE StadiVari'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1622
_diffrn_reflns_av_unetI/netI     0.2289
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            38479
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.190
_diffrn_source                   'Genix 3D HF Mo'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.484
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.899
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'STOE X-AREA 1.76'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.078
_exptl_crystal_description       block
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.758
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.894
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     503
_refine_ls_number_reflns         9847
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.894
_refine_ls_R_factor_all          0.2087
_refine_ls_R_factor_gt           0.0772
_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^)+(0.1144P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1869
_refine_ls_wR_factor_ref         0.2419
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3922
_reflns_number_total             9847
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc03516j2.cif
_cod_data_source_block           2b_prime
_cod_depositor_comments
'Adding full bibliography for 1572143--1572150.cif.'
_cod_original_cell_volume        5038.9(18)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C22.50 H34 N2 Ni0.50 O P'
_cod_database_code               1572146
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              99378
_shelx_hkl_checksum              13398