Structural, magnetic and photoluminescence properties of new hybrid hypophosphites: discovery of the first noncentrosymmetric and two cobalt-based members
Mączka, Mirosław; Gągor, Anna; Stefańska, Dagmara; Zaręba, Jan K.; Pikul, Adam; Dalton Transactions  (2022) –; doi:10.1039/D2DT01212J

data_7710408
_publ_section_title
;
 Structural, magnetic and photoluminescence properties of new hybrid
 hypophosphites: discovery of the first noncentrosymmetric and two
 cobalt-based members
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01212J
_journal_year                    2022
_chemical_formula_moiety         'Cd1 H6 O6 P3, C1 H6 N3'
_chemical_formula_sum            'C H12 Cd N3 O6 P3'
_chemical_formula_weight         367.45
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-01-19
_audit_creation_method
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_audit_update_record
;
2022-02-21 deposited with the CCDC.	2022-05-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   9.2500(2)
_cell_length_b                   9.2500(2)
_cell_length_c                   23.0532(6)
_cell_measurement_reflns_used    7508
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.1170
_cell_measurement_theta_min      3.0610
_cell_volume                     1708.23(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6249
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -71.00  71.00   1.00    2.60    --   13.31 -19.00  90.00  142
  2  \w    -25.00  30.00   1.00    2.60    --  -14.40 -99.00 -90.00   55
  3  \w    -47.00  64.00   1.00    2.60    --  -14.40  57.00 -60.00  111
  4  \w    -92.00  18.00   1.00    2.60    --  -14.40 -57.00  30.00  110
  5  \w     35.00 106.00   1.00    2.60    --   13.31 178.00 150.00   71
  6  \w    -25.00  57.00   1.00    2.60    --   13.31 -99.00-180.00   82
  7  \w    -25.00  57.00   1.00    2.60    --   13.31 -99.00  60.00   82
  8  \w   -105.00 -32.00   1.00    2.60    --  -14.40 178.00  90.00   73
  9  \w    -25.00   2.00   1.00    2.60    --  -14.40 -99.00  90.00   27
 10  \w    -94.00  17.00   1.00    2.60    --  -14.40 -37.00 150.00  111
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0113905333
_diffrn_orient_matrix_UB_12      0.0436578667
_diffrn_orient_matrix_UB_13      0.0264399667
_diffrn_orient_matrix_UB_21      0.0861360000
_diffrn_orient_matrix_UB_22      0.0511470000
_diffrn_orient_matrix_UB_23      -0.0063455000
_diffrn_orient_matrix_UB_31      -0.0170498667
_diffrn_orient_matrix_UB_32      0.0576076667
_diffrn_orient_matrix_UB_33      -0.0144025333
_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  0.0314
_diffrn_reflns_av_unetI/netI     0.0121
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            11397
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.525
_diffrn_reflns_theta_min         3.097
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.347
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89709
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    2.143
_exptl_crystal_description       plate
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.533
_refine_diff_density_min         -0.744
_refine_diff_density_rms         0.083
_refine_ls_extinction_coef       0.0171(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     29
_refine_ls_number_reflns         523
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0199
_refine_ls_R_factor_gt           0.0184
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0250P)^2^+4.0349P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0441
_refine_ls_wR_factor_ref         0.0450
_reflns_Friedel_coverage         0.000
_reflns_number_gt                494
_reflns_number_total             523
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01212j2.cif
_cod_data_source_block           gua_cdpo2_1792d
_cod_original_cell_volume        1708.23(9)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               7710408
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         N3C1P3O12H6Cd
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
2. Others
 Fixed Sof: H1A(0.5) H1B(0.5)
3.a X=CH2 refined with riding coordinates:
 N1(H1A,H1B)
;
_shelx_res_checksum              99412
_shelx_hkl_checksum              24241
_olex2_date_sample_data_collection 2020-07-16
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.095
_oxdiff_exptl_absorpt_empirical_full_min 0.931