PCP and POCOP complexes of calcium
Messori, Alessandro; Potocnik, Marcel; Belazregue, Sara; Collins, Richard; Krämer, Tobias; Chadwick, F. Mark; Chemical Communications 61 (2025) 7827–7830; doi:10.1039/D5CC00872G

data_7134464
_publ_section_title
;
 PCP and POCOP complexes of calcium
;
_journal_issue                   43
_journal_name_full               'Chemical Communications'
_journal_page_first              7827
_journal_page_last               7830
_journal_paper_doi               10.1039/D5CC00872G
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C30 H60 Ca N P2 Si2'
_chemical_formula_sum            'C30 H60 Ca N P2 Si2'
_chemical_formula_weight         592.99
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-11-10
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2025-02-12 deposited with the CCDC.	2025-03-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.6480(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.4016(2)
_cell_length_b                   14.4612(2)
_cell_length_c                   20.6761(3)
_cell_measurement_reflns_used    7297
_cell_measurement_temperature    173.00
_cell_measurement_theta_max      73.5420
_cell_measurement_theta_min      3.7100
_cell_volume                     3695.90(10)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4115
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.965
_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    -67.00  32.00   1.00    2.00    --  -42.36  38.00  90.00   99
  2  \w    -98.00  -2.00   1.00    2.00    --  -42.36 125.00  90.00   96
  3  \w     36.00 111.00   1.00    4.00    --  105.75 -45.00-150.00   75
  4  \w    101.00 155.00   1.00    4.00    --  105.75  45.00 -30.00   54
  5  \w    128.00 168.00   1.00    4.00    --  105.75  45.00-150.00   40
  6  \w     32.00 107.00   1.00    4.00    --  105.75 -30.00  30.00   75
  7  \w     35.00 105.00   1.00    4.00    --  105.75 -95.00   0.00   70
  8  \w     23.00 109.00   1.00    4.00    --  105.75 -95.00-150.00   86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1222739000
_diffrn_orient_matrix_UB_12      -0.0111174000
_diffrn_orient_matrix_UB_13      0.0180987000
_diffrn_orient_matrix_UB_21      -0.0139490000
_diffrn_orient_matrix_UB_22      -0.1058476000
_diffrn_orient_matrix_UB_23      0.0018949000
_diffrn_orient_matrix_UB_31      0.0197248000
_diffrn_orient_matrix_UB_32      -0.0056625000
_diffrn_orient_matrix_UB_33      -0.0724695000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            13735
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.680
_diffrn_reflns_theta_min         3.576
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.021
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64461
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.066
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1300
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.490
_refine_diff_density_min         -0.501
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         7220
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0398
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0674P)^2^+1.0888P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1057
_refine_ls_wR_factor_ref         0.1153
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6234
_reflns_number_total             7220
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc00872g2.cif
_cod_data_source_block           fmc2231
_cod_depositor_comments
'Adding full bibliography for 7134464--7134468.cif.'
_cod_database_code               7134464
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.864
_shelx_estimated_absorpt_t_min   0.583
_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.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C00O(H00D,H00E)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C4(H4)
2.c Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C00K(H00A,H00B,H00C), C20(H20A,H20B,H20C), C22(H22A,H22B,
 H22C), C18(H18A,H18B,H18C), C14(H14A,H14B,H14C), C00Q(H00F,H00G,H00H),
 C19(H19A,H19B,H19C), C15(H15A,H15B,H15C), C24(H24A,H24B,H24C), C00U(H00I,H00J,
 H00K), C16(H16A,H16B,H16C), C00W(H00L,H00M,H00N), C00X(H00O,H00P,H00Q),
 C12(H12A,H12B,H12C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C)
;
_shelx_res_checksum              53892
_shelx_hkl_checksum              69055
_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 1.431
_oxdiff_exptl_absorpt_empirical_full_min 0.783