#------------------------------------------------------------------------------
#$Date: 2022-11-07 07:39:49 +0200 (Mon, 07 Nov 2022) $
#$Revision: 279011 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/06/17/7061793.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7061793
loop_
_publ_author_name
'Kelly, Jordan C.'
'Bloomfield, Aaron J.'
_publ_section_title
;
 High-spin, tetrahedral cobalt(ii) and nickel(ii) complexes supported by
 monoprotic aminophosphine ligands, and attempted extension to copper(ii)
 complexes: synthesis, characterization, and unexpected reactivity
;
_journal_issue                   39
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              18647
_journal_page_last               18651
_journal_paper_doi               10.1039/D2NJ02651A
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C30 H54 Cl4 Cu2 N4 O2 P2'
_chemical_formula_sum            'C30 H54 Cl4 Cu2 N4 O2 P2'
_chemical_formula_weight         833.59
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/ccdc.csd.cc2bs6zb
_audit_creation_date             2022-08-05
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-08-08 deposited with the CCDC.	2022-09-05 downloaded from the CCDC.
;
_cell_angle_alpha                110.5230(10)
_cell_angle_beta                 101.0310(10)
_cell_angle_gamma                109.1720(10)
_cell_formula_units_Z            1
_cell_length_a                   8.3490(4)
_cell_length_b                   11.6402(6)
_cell_length_c                   11.6734(6)
_cell_measurement_reflns_used    8858
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.5069
_cell_measurement_theta_min      2.6384
_cell_volume                     941.38(8)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'Bruker Instrument Service V2017.5.0.0'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.899
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0155
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.899
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12243
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.899
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.789
_diffrn_reflns_theta_min         2.069
_diffrn_source                   'fine focus sealed tube X-ray source'
_exptl_absorpt_coefficient_mu    1.531
_exptl_absorpt_correction_T_max  0.770
_exptl_absorpt_correction_T_min  0.450
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular prism'
_exptl_crystal_F_000             434
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.513
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         6271
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0221
_refine_ls_R_factor_gt           0.0203
_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/[σ²(Fo²)+(0.0287P)²+0.2861P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0560
_refine_ls_wR_factor_ref         0.0567
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5880
_reflns_number_total             6271
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2nj02651a2.cif
_cod_data_source_block           JCK_CutBu2C_teal_01292021
_cod_depositor_comments
'Adding full bibliography for 7061787--7061798.cif.'
_cod_database_code               7061793
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.770
_shelx_estimated_absorpt_t_min   0.450
_exptl_absorpt_special_details   mu*r=0.2000
_olex2_refinement_description
;
1. Restrained distances
 N2-H2N
 0.9 with sigma of 0.02
 P1-H2N
 2.12 with sigma of 0.04
 C7-H2N
 1.95 with sigma of 0.04
2.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4)
2.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,
 H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.18959(2) 0.20615(2) 0.43160(2) 0.01336(4) Uani 1 1 d . . . . .
Cl1 Cl 0.08428(4) 0.32261(3) 0.57114(2) 0.02290(5) Uani 1 1 d . . . . .
Cl2 Cl 0.10996(3) 0.00359(2) 0.26693(2) 0.01942(5) Uani 1 1 d . . . . .
P1 P 0.14889(3) 0.36572(2) 0.24209(2) 0.01250(5) Uani 1 1 d D . . . .
O1 O 0.20477(10) 0.30152(8) 0.32458(7) 0.01841(13) Uani 1 1 d . . . . .
N1 N 0.66320(11) 0.82721(8) 0.43922(8) 0.01455(14) Uani 1 1 d . . . . .
N2 N 0.20386(11) 0.52866(8) 0.33156(8) 0.01599(15) Uani 1 1 d D . . . .
C1 C 0.74031(15) 0.87564(11) 0.36444(10) 0.01953(18) Uani 1 1 d . . . . .
H1 H 0.856536 0.884399 0.369343 0.023 Uiso 1 1 calc R U . . .
C2 C 0.65217(17) 0.91280(12) 0.28052(11) 0.0244(2) Uani 1 1 d . . . . .
H2 H 0.708313 0.946345 0.230109 0.029 Uiso 1 1 calc R U . . .
C3 C 0.47843(17) 0.89899(12) 0.27311(11) 0.0254(2) Uani 1 1 d . . . . .
H3 H 0.416695 0.923983 0.218143 0.031 Uiso 1 1 calc R U . . .
C4 C 0.39801(15) 0.84740(11) 0.34880(11) 0.02125(19) Uani 1 1 d . . . . .
H4 H 0.280995 0.836238 0.343950 0.026 Uiso 1 1 calc R U . . .
C5 C 0.49347(13) 0.81246(9) 0.43202(9) 0.01497(16) Uani 1 1 d . . . . .
C6 C 0.41091(13) 0.75519(10) 0.51477(9) 0.01642(17) Uani 1 1 d . . . . .
H6A H 0.308378 0.775666 0.521088 0.020 Uiso 1 1 calc R U . . .
H6B H 0.499048 0.799403 0.602038 0.020 Uiso 1 1 calc R U . . .
C7 C 0.34802(13) 0.60140(10) 0.46103(9) 0.01622(16) Uani 1 1 d D . . . .
H7A H 0.449717 0.580060 0.453858 0.019 Uiso 1 1 calc R U . . .
H7B H 0.303057 0.571148 0.520966 0.019 Uiso 1 1 calc R U . . .
C8 C 0.27851(14) 0.35563(10) 0.12983(10) 0.01721(17) Uani 1 1 d . . . . .
C9 C 0.47559(15) 0.46035(12) 0.21227(12) 0.0254(2) Uani 1 1 d . . . . .
H9A H 0.549340 0.454729 0.158578 0.038 Uiso 1 1 calc R U . . .
H9B H 0.519243 0.441540 0.282743 0.038 Uiso 1 1 calc R U . . .
H9C H 0.480988 0.550043 0.246846 0.038 Uiso 1 1 calc R U . . .
C10 C 0.21149(19) 0.38940(15) 0.01972(13) 0.0318(3) Uani 1 1 d . . . . .
H10A H 0.292595 0.393441 -0.028530 0.048 Uiso 1 1 calc R U . . .
H10B H 0.207068 0.475681 0.056072 0.048 Uiso 1 1 calc R U . . .
H10C H 0.092787 0.320268 -0.037425 0.048 Uiso 1 1 calc R U . . .
C11 C 0.27408(16) 0.21329(12) 0.07223(12) 0.0254(2) Uani 1 1 d . . . . .
H11A H 0.153760 0.147795 0.014603 0.038 Uiso 1 1 calc R U . . .
H11B H 0.309801 0.190660 0.141532 0.038 Uiso 1 1 calc R U . . .
H11C H 0.355898 0.212614 0.024602 0.038 Uiso 1 1 calc R U . . .
C12 C -0.09821(13) 0.28685(10) 0.16043(9) 0.01598(16) Uani 1 1 d . . . . .
C13 C -0.18162(15) 0.28901(12) 0.26736(11) 0.0236(2) Uani 1 1 d . . . . .
H13A H -0.311047 0.246423 0.228761 0.035 Uiso 1 1 calc R U . . .
H13B H -0.142083 0.381361 0.329843 0.035 Uiso 1 1 calc R U . . .
H13C H -0.143807 0.240590 0.310203 0.035 Uiso 1 1 calc R U . . .
C14 C -0.16114(15) 0.13798(11) 0.06331(11) 0.0238(2) Uani 1 1 d . . . . .
H14A H -0.290690 0.092102 0.032602 0.036 Uiso 1 1 calc R U . . .
H14B H -0.110813 0.094142 0.105818 0.036 Uiso 1 1 calc R U . . .
H14C H -0.121233 0.134666 -0.009156 0.036 Uiso 1 1 calc R U . . .
C15 C -0.16275(16) 0.36275(12) 0.09165(12) 0.0250(2) Uani 1 1 d . . . . .
H15A H -0.113239 0.360748 0.023592 0.037 Uiso 1 1 calc R U . . .
H15B H -0.122985 0.455341 0.153635 0.037 Uiso 1 1 calc R U . . .
H15C H -0.292347 0.319597 0.054745 0.037 Uiso 1 1 calc R U . . .
H2N H 0.1134(19) 0.5474(16) 0.3338(15) 0.030 Uiso 1 1 d D U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl2 Cu1 Cl1 142.477(11) . . ?
O1 Cu1 Cl1 98.83(2) . . ?
O1 Cu1 Cl2 94.72(2) . . ?
O1 Cu1 N1 143.43(3) . 2_666 ?
N1 Cu1 Cl1 95.58(2) 2_666 . ?
N1 Cu1 Cl2 93.93(2) 2_666 . ?
O1 P1 N2 111.61(4) . . ?
O1 P1 C8 106.09(4) . . ?
O1 P1 C12 111.90(4) . . ?
N2 P1 C8 107.79(5) . . ?
N2 P1 C12 105.05(4) . . ?
C12 P1 C8 114.43(5) . . ?
P1 O1 Cu1 159.31(5) . . ?
C1 N1 Cu1 118.71(7) . 2_666 ?
C1 N1 C5 119.57(9) . . ?
C5 N1 Cu1 121.51(7) . 2_666 ?
P1 N2 H2N 114.3(11) . . ?
C7 N2 P1 118.51(6) . . ?
C7 N2 H2N 111.9(10) . . ?
N1 C1 H1 118.9 . . ?
N1 C1 C2 122.16(10) . . ?
C2 C1 H1 118.9 . . ?
C1 C2 H2 120.6 . . ?
C1 C2 C3 118.71(10) . . ?
C3 C2 H2 120.6 . . ?
C2 C3 H3 120.4 . . ?
C4 C3 C2 119.15(10) . . ?
C4 C3 H3 120.4 . . ?
C3 C4 H4 120.2 . . ?
C3 C4 C5 119.64(10) . . ?
C5 C4 H4 120.2 . . ?
N1 C5 C4 120.75(9) . . ?
N1 C5 C6 117.89(8) . . ?
C4 C5 C6 121.35(9) . . ?
C5 C6 H6A 109.0 . . ?
C5 C6 H6B 109.0 . . ?
C5 C6 C7 113.12(8) . . ?
H6A C6 H6B 107.8 . . ?
C7 C6 H6A 109.0 . . ?
C7 C6 H6B 109.0 . . ?
N2 C7 C6 111.00(8) . . ?
N2 C7 H7A 109.4 . . ?
N2 C7 H7B 109.4 . . ?
C6 C7 H7A 109.4 . . ?
C6 C7 H7B 109.4 . . ?
H7A C7 H7B 108.0 . . ?
C9 C8 P1 106.72(7) . . ?
C10 C8 P1 113.41(8) . . ?
C10 C8 C9 108.35(10) . . ?
C10 C8 C11 109.88(9) . . ?
C11 C8 P1 109.81(7) . . ?
C11 C8 C9 108.52(9) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C13 C12 P1 106.53(7) . . ?
C14 C12 P1 109.29(7) . . ?
C14 C12 C13 108.30(9) . . ?
C15 C12 P1 113.38(7) . . ?
C15 C12 C13 108.66(9) . . ?
C15 C12 C14 110.49(9) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 Cl1 2.2465(3) . ?
Cu1 Cl2 2.2361(3) . ?
Cu1 O1 1.9364(7) . ?
Cu1 N1 1.9876(8) 2_666 ?
P1 O1 1.5050(7) . ?
P1 N2 1.6597(9) . ?
P1 C8 1.8494(10) . ?
P1 C12 1.8432(10) . ?
N1 C1 1.3475(13) . ?
N1 C5 1.3524(12) . ?
N2 C7 1.4788(12) . ?
N2 H2N 0.854(12) . ?
C1 H1 0.9300 . ?
C1 C2 1.3852(15) . ?
C2 H2 0.9300 . ?
C2 C3 1.3880(17) . ?
C3 H3 0.9300 . ?
C3 C4 1.3878(17) . ?
C4 H4 0.9300 . ?
C4 C5 1.3922(14) . ?
C5 C6 1.5024(14) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C7 1.5306(13) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C9 1.5406(15) . ?
C8 C10 1.5308(15) . ?
C8 C11 1.5387(15) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 C13 1.5381(14) . ?
C12 C14 1.5366(14) . ?
C12 C15 1.5363(14) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
