Synthesis, crystal structures and magnetic properties of a P-stereogenic <i>ortho</i>-(4-amino-tempo)phosphinic amide radical and its Cu<sup>II</sup> complex.
Navarro, Yolanda; Guedes, Guilherme P.; Del Águila-Sánchez, Miguel A; Iglesias, María José; Lloret, Francisco; López-Ortiz, Fernando; Dalton transactions (Cambridge, England : 2003) 50 (2021) 2585–2595; doi:10.1039/d0dt04298f

data_7706427
_publ_section_title
;
 Synthesis, crystal structures and magnetic properties of a P-stereogenic
 <i>ortho</i>-(4-amino-tempo)phosphinic amide radical and its
 Cu<sup>II</sup> complex.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2585
_journal_page_last               2595
_journal_paper_doi               10.1039/d0dt04298f
_journal_volume                  50
_journal_year                    2021
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C27 H41 N3 O2 P'
_chemical_formula_sum            'C27 H41 N3 O2 P'
_chemical_formula_weight         470.60
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2020-08-24
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2020-08-24 deposited with the CCDC.	2021-01-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.3792(2)
_cell_length_b                   17.0809(4)
_cell_length_c                   18.6707(4)
_cell_measurement_reflns_used    8112
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      74.18
_cell_measurement_theta_min      3.51
_cell_volume                     2672.23(11)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_unetI/netI     0.0442
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.941
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            13459
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.164
_diffrn_reflns_theta_min         3.507
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.117
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8239
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1718 before and 0.0804 after correction.
The Ratio of minimum to maximum transmission is 0.4973.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.170
_exptl_crystal_description       block
_exptl_crystal_F_000             1020
_exptl_crystal_size_max          0.228
_exptl_crystal_size_mid          0.129
_exptl_crystal_size_min          0.098
_refine_diff_density_max         0.208
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details
;
 Flack x determined using 1907 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.024(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         5071
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0300
_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^)+(0.0369P)^2^+0.1130P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0719
_refine_ls_wR_factor_ref         0.0750
_reflns_Friedel_coverage         0.747
_reflns_Friedel_fraction_full    0.971
_reflns_Friedel_fraction_max     0.921
_reflns_number_gt                4679
_reflns_number_total             5437
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt04298f2.cif
_cod_data_source_block           yn36_0m_a
_cod_depositor_comments
'Adding full bibliography for 7706427--7706428.cif.'
_cod_database_code               7706427
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C22(H22), C5(H5)
2.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C4(H4A,H4B)
2.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C17(H17), C12(H12), C20(H20), C11(H11), C14(H14), C18(H18),
 C21(H21), C19(H19)
2.d Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C9(H9A,H9B,H9C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C),
 C8(H8A,H8B,H8C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C23(H23A,H23B,H23C)
;
_shelx_res_checksum              71118
_olex2_submission_special_instructions 'No special instructions were received'
_publcif_funding_html
;
;