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_7704127
_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         '0.5(C144 H144 Cr2 K4 N16 O8 P8)'
_chemical_formula_sum            'C72 H72 Cr K2 N8 O4 P4'
_chemical_formula_weight         1367.46
_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                 101.428(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.1285(18)
_cell_length_b                   16.1863(11)
_cell_length_c                   18.8547(10)
_cell_measurement_reflns_used    3913
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.1560
_cell_measurement_theta_min      3.2720
_cell_volume                     7217.7(8)
_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
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      298(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0251
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9976
_diffrn_measured_fraction_theta_max 0.8656
_diffrn_measurement_details
;
  1 omega   35.00   88.00   1.0000   57.8050
omega____ theta____ kappa____ phi______ frames
    -       15.5265  178.0000   30.0000 53

  2 omega  -25.00   22.00   1.0000   57.8050
omega____ theta____ kappa____ phi______ frames
    -      -17.0890  -99.0000 -150.0000 47

  3 omega  -84.00    0.00   1.0000   57.8050
omega____ theta____ kappa____ phi______ frames
    -      -17.0890  -57.0000   30.0000 84

  4 omega  -88.00   12.00   1.0000   57.8050
omega____ theta____ kappa____ phi______ frames
    -      -17.0890  -19.0000   90.0000 100

  5 omega  -52.00  -27.00   1.0000   57.8050
omega____ theta____ kappa____ phi______ frames
    -       15.5265  -77.0000  150.0000 25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0215296000
_diffrn_orient_matrix_UB_12      -0.0142338000
_diffrn_orient_matrix_UB_13      -0.0286476000
_diffrn_orient_matrix_UB_21      -0.0202012000
_diffrn_orient_matrix_UB_22      0.0043609000
_diffrn_orient_matrix_UB_23      0.0224177000
_diffrn_orient_matrix_UB_31      -0.0052879000
_diffrn_orient_matrix_UB_32      0.0412193000
_diffrn_orient_matrix_UB_33      -0.0122402000
_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  0.0788
_diffrn_reflns_av_unetI/netI     0.1074
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            20006
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.05
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 1.0000
_diffrn_standards_interval_time  57.8050
_diffrn_standards_number         23877
_exptl_absorpt_coefficient_mu    0.415
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.25119
_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            colourless
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2856
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.760
_refine_diff_density_min         -0.435
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         6602
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.1513
_refine_ls_R_factor_gt           0.0776
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1176P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1955
_refine_ls_wR_factor_ref         0.2488
_reflns_number_gt                3102
_reflns_number_total             6602
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d0dt00878h2.cif
_cod_data_source_block           exp_294
_cod_depositor_comments
'Adding full bibliography for 7704126--7704127.cif.'
_cod_database_code               7704127
_reflns_odcompleteness_completeness 99.76
_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
2. Restrained distances
 C34-C35
 1.5 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C33 \\sim C34 \\sim C35 \\sim C36: within 1.7A with sigma of 0.005 and sigma for terminal atoms of 0.005
C29 \\sim C30 \\sim C31 \\sim C32: within 1.7A with sigma of 0.005 and sigma for terminal atoms of 0.005
4.a Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,
 H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C24(H24),
  C25(H25), C26(H26), C27(H27), C28(H28)
;