Cyclo-Tetrakis(μ-diphenylphosphido)-1,5-bis(tri-tert-butylphosphine)-Tetracopper
Dannenberg, Steven G.; Waterman, Rory; Molbank 2022 (2022) M1334–; doi:10.3390/M1334

data_1566568
_publ_section_title
;
 Cyclo-Tetrakis(\m-diphenylphosphido)-1,5-bis(tri-tert-butylphosphine)-Tetracopper
;
_journal_issue                   1
_journal_name_full               Molbank
_journal_page_first              M1334
_journal_paper_doi               10.3390/M1334
_journal_volume                  2022
_journal_year                    2022
_chemical_formula_moiety         'C72 H94 Cu4 P6, 2(C4 H8 O)'
_chemical_formula_sum            'C80 H110 Cu4 O2 P6'
_chemical_formula_weight         1543.65
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
FinalCif V95 by Daniel Kratzert, Freiburg 2021,
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2021-12-27 deposited with the CCDC.	2022-01-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.715(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.127(10)
_cell_length_b                   19.946(11)
_cell_length_c                   23.841(14)
_cell_measurement_reflns_used    9881
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.3245
_cell_measurement_theta_min      2.3865
_cell_volume                     7840(8)
_computing_cell_refinement       'SAINT V8.37A'
_computing_data_collection
'Bruker BIS 2016.5.0.1/14-Jun-2016 && APEX3_2016.5-0'
_computing_data_reduction        'SAINT V8.37A'
_computing_molecular_graphics    'ShelXle (Hu\"bschle 2011)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w''
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0881
_diffrn_reflns_av_unetI/netI     0.0587
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            90959
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.504
_diffrn_reflns_theta_min         1.662
_diffrn_source_current           30.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.236
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.6
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction:
Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48
(2015) 3-10
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3248
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: pentane'
_exptl_crystal_size_max          0.466
_exptl_crystal_size_mid          0.232
_exptl_crystal_size_min          0.112
_refine_diff_density_max         0.478
_refine_diff_density_min         -0.467
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.951
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     847
_refine_ls_number_reflns         17898
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.951
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0332
_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^)+(0.0417P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0787
_refine_ls_wR_factor_ref         0.0839
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13043
_reflns_number_total             17898
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            s5.cif
_cod_data_source_block           SD421012621_0m
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1566568
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.597
_shelx_estimated_absorpt_t_max   0.874
_diffrn_measurement_ambient_temperature_device_make 'Oxford Cryostream 700'
_shelx_res_checksum              8971
_shelx_hkl_checksum              9757