1,2-Diaza-4-phospholide complexes of chromium(ii): dipotassium organochromates behaving as single-molecule magnets.
Su, Jing; Yin, Lei; Ouyang, Zhongwen; Wang, Zhenxing; Zheng, Wenjun; Dalton transactions (Cambridge, England : 2003) 49 (2020) 6945–6949; doi:10.1039/d0dt00878h

data_7704126
_publ_section_title
;
 1,2-Diaza-4-phospholide complexes of chromium(ii): dipotassium
 organochromates behaving as single-molecule magnets.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6945
_journal_page_last               6949
_journal_paper_doi               10.1039/d0dt00878h
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C56 H104 Cr K2 N8 O4 P4, 0.5(C14 H16)'
_chemical_formula_sum            'C63 H112 Cr K2 N8 O4 P4'
_chemical_formula_weight         1299.69
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-05-27
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_audit_update_record
;
2018-06-11 deposited with the CCDC.	2020-04-17 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 93.463(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.4723(9)
_cell_length_b                   24.2440(9)
_cell_length_c                   19.1309(6)
_cell_measurement_reflns_used    4098
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.2280
_cell_measurement_theta_min      3.5660
_cell_volume                     7626.1(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
'SUPERFLIP, J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0251
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9981
_diffrn_measured_fraction_theta_max 0.8414
_diffrn_measurement_details
;
  1 omega  -31.00    0.00   1.0000    9.5750
omega____ theta____ kappa____ phi______ frames
    -      -17.1671   57.0000  -90.0000 31

  2 omega  -36.00   44.00   1.0000    9.5750
omega____ theta____ kappa____ phi______ frames
    -      -17.1671   37.0000 -150.0000 80

  3 omega  -48.00   22.00   1.0000    9.5750
omega____ theta____ kappa____ phi______ frames
    -       15.6827  -57.0000   30.0000 70

  4 omega  -11.00   18.00   1.0000    9.5750
omega____ theta____ kappa____ phi______ frames
    -      -17.1671  -99.0000 -150.0000 29

  5 omega  -18.00   17.00   1.0000    9.5750
omega____ theta____ kappa____ phi______ frames
    -      -17.1671  -99.0000   30.0000 35
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0067009000
_diffrn_orient_matrix_UB_12      -0.0258548000
_diffrn_orient_matrix_UB_13      -0.0160266000
_diffrn_orient_matrix_UB_21      0.0298376000
_diffrn_orient_matrix_UB_22      0.0121948000
_diffrn_orient_matrix_UB_23      -0.0203109000
_diffrn_orient_matrix_UB_31      0.0304236000
_diffrn_orient_matrix_UB_32      -0.0062641000
_diffrn_orient_matrix_UB_33      0.0266413000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            19185
_diffrn_reflns_theta_full        26.34
_diffrn_reflns_theta_max         26.34
_diffrn_reflns_theta_min         2.97
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 1
_diffrn_standards_interval_time  9.5750
_diffrn_standards_number         20744
_exptl_absorpt_coefficient_mu    0.388
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84945
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.132
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2800
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.447
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         7808
_refine_ls_number_restraints     47
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0918
_refine_ls_R_factor_gt           0.0537
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0826P)^2^+3.5465P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1407
_refine_ls_wR_factor_ref         0.1636
_reflns_number_gt                5104
_reflns_number_total             7808
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d0dt00878h2.cif
_cod_data_source_block           exp_82
_cod_depositor_comments
'Adding full bibliography for 7704126--7704127.cif.'
_cod_original_cell_volume        7626.0(5)
_cod_database_code               7704126
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{O1, O1'}
3. Restrained distances
 C25'-O1' \\sim C28'-O1'
 with sigma of 0.01
 C25-O1 \\sim C28-O1
 with sigma of 0.01
 C25-C26 \\sim C26-C27 \\sim C27-C28
 with sigma of 0.01
 C25'-C26' \\sim C26'-C27' \\sim C27'-C28'
 with sigma of 0.01
 C26'-O1' \\sim C27'-O1'
 with sigma of 0.01
 C26-O1 \\sim C27-O1
 with sigma of 0.01
4. Rigid bond restraints
 O2, C21
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Uiso/Uaniso restraints and constraints
C25' \\sim C26' \\sim C27' \\sim C28': within 1.7A with sigma of 0.005 and sigma for terminal atoms of 0.005
C25 \\sim C26 \\sim C27 \\sim C28: within 1.7A with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(O1) = Uanis(O1')
6. Others
 Sof(C25')=Sof(H25C)=Sof(H25D)=Sof(C26')=Sof(H26C)=Sof(H26D)=Sof(C27')=
 Sof(H27C)=Sof(H27D)=Sof(C28')=Sof(H28C)=Sof(H28D)=Sof(O1')=1-FVAR(1)
 Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(C27)=Sof(H27A)=
 Sof(H27B)=Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(O1)=FVAR(1)
 Uiso(C29)=Uiso(C30)=Uiso(C31)=Uiso(C32)=Uiso(C33)=Uiso(C34)=Uiso(C35)=FVAR(2)
 Fixed Sof: C29(0.5) H29A(0.5) C30(0.5) H30A(0.5) C31(0.5) H31A(0.5) C32(0.5)
 H32A(0.5) C33(0.5) H33A(0.5) C34(0.5) C35(0.5) H35A(0.5) H35B(0.5) H35C(0.5)
7.a Riding coordinates:
 C29(H29A,C30), C29(H30A,C31), C29(H31A,C32), C29(H32A,C33), C29(H33A,C34,C35),
  C29(H35A,H35B,H35C)
7.b Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,
 H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C25'(H25C,H25D),
 C26'(H26C,H26D), C27'(H27C,H27D), C28'(H28C,H28D)
7.c Fitted hexagon refined as free rotating group:
 C29(C25',C26',C27',C28',Cr1)
7.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C9(H9A,
 H9B,H9C), C10(H10A,H10B,H10C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C),
 C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C)
;
_olex2_submission_special_instructions 'No special instructions were received'