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_7710406
_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         'Co H6 O6 P3, C H6 N3'
_chemical_formula_sum            'C H12 Co N3 O6 P3'
_chemical_formula_weight         313.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-I 2y'
_space_group_name_H-M_alt        'I 1 2/m 1'
_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                 90.623(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.6597(4)
_cell_length_b                   13.0778(6)
_cell_length_c                   9.4000(5)
_cell_measurement_reflns_used    3073
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.3290
_cell_measurement_theta_min      2.8000
_cell_volume                     1064.49(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 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, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_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 0.907
_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     32.00 104.00   1.20    5.00    --   13.31-178.00  30.00   60
  2  \w    -25.00  29.00   1.20    5.00    --  -14.40 -99.00 -90.00   45
  3  \w    -46.00  63.20   1.20    5.00    --  -14.40  57.00  60.00   91
  4  \w    -19.00   5.00   1.20    5.00    --   13.31  57.00 150.00   20
  5  \w    -46.00  64.40   1.20    5.00    --  -14.40  37.00-150.00   92
;
_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      0.0179701000
_diffrn_orient_matrix_UB_12      0.0088257000
_diffrn_orient_matrix_UB_13      -0.0724265000
_diffrn_orient_matrix_UB_21      0.0758161000
_diffrn_orient_matrix_UB_22      -0.0188101000
_diffrn_orient_matrix_UB_23      0.0122455000
_diffrn_orient_matrix_UB_31      -0.0253144000
_diffrn_orient_matrix_UB_32      -0.0500848000
_diffrn_orient_matrix_UB_33      -0.0173200000
_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  0.0210
_diffrn_reflns_av_unetI/netI     0.0206
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.907
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5023
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.907
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.331
_diffrn_reflns_theta_min         2.669
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.072
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94467
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.959
_exptl_crystal_description       plate
_exptl_crystal_F_000             636
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.510
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       0.0231(9)
_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   1.095
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     86
_refine_ls_number_reflns         1379
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0231
_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^)+(0.0288P)^2^+0.9483P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0582
_refine_ls_wR_factor_ref         0.0615
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1246
_reflns_number_total             1379
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01212j2.cif
_cod_data_source_block           guacopo2_rt
_cod_database_code               7710406
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CoP3O6NC3
_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), N2(H2C,H2D)
;
_shelx_res_checksum              619
_shelx_hkl_checksum              30189
_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 1.122
_oxdiff_exptl_absorpt_empirical_full_min 0.933