On the existence of low-valent magnesium-calcium complexes.
Mai, Jonathan; Rösch, Bastian; Patel, Neha; Langer, Jens; Harder, Sjoerd; Chemical science 14 (2023) 4724–4734; doi:10.1039/d3sc00909b

data_1568860
_publ_section_title
;
 On the existence of low-valent magnesium-calcium complexes.
;
_journal_issue                   18
_journal_name_full               'Chemical science'
_journal_page_first              4724
_journal_page_last               4734
_journal_paper_doi               10.1039/d3sc00909b
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C82 H132 Ca2 N4 O2, C6 H14, 1[C6H14]'
_chemical_formula_sum            'C94 H160 Ca2 N4 O2'
_chemical_formula_weight         1458.41
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-11-11
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-02-08 deposited with the CCDC.	2023-04-13 downloaded from the CCDC.
;
_cell_angle_alpha                74.198(4)
_cell_angle_beta                 73.222(4)
_cell_angle_gamma                63.566(4)
_cell_formula_units_Z            1
_cell_length_a                   12.4506(6)
_cell_length_b                   12.9760(6)
_cell_length_c                   16.2431(6)
_cell_measurement_reflns_used    10418
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      72.8440
_cell_measurement_theta_min      3.8330
_cell_volume                     2217.94(19)
_computing_cell_refinement       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.971
_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   -114.00 -13.00   1.00    3.00    --  -41.15 -57.00  90.00  101
  2  \w    -69.00  32.00   1.00    3.00    --  -41.15  57.00-120.00  101
  3  \w    -66.00  33.00   1.00    3.00    --  -41.15  38.00  30.00   99
  4  \w     23.00  97.00   1.00    3.00    --   41.15-125.00  30.00   74
  5  \w     33.00 134.00   1.00   12.00    --  104.96 -61.00  60.00  101
  6  \w     72.00 178.00   1.00   12.00    --  104.96  77.00   0.00  106
  7  \w     29.00 138.00   1.00   12.00    --  104.96 -77.00-150.00  109
  8  \w     32.00 131.00   1.00   12.00    --  104.96 -45.00-150.00   99
  9  \w     35.00 128.00   1.00   12.00    --  104.96 -45.00 -60.00   93
 10  \w     42.00 121.00   1.00   12.00    --  104.96-125.00-120.00   79
 11  \w     60.00 106.00   1.00   12.00    --  104.96 -94.00  60.00   46
 12  \w     71.00 109.00   1.00   12.00    --  104.96 -94.00 -30.00   38
 13  \w     18.00 174.00   1.00   12.00    --  104.96   0.00   0.00  156
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0621831000
_diffrn_orient_matrix_UB_12      0.0096520000
_diffrn_orient_matrix_UB_13      -0.0970273000
_diffrn_orient_matrix_UB_21      0.1013738000
_diffrn_orient_matrix_UB_22      -0.1219324000
_diffrn_orient_matrix_UB_23      0.0190950000
_diffrn_orient_matrix_UB_31      -0.0754990000
_diffrn_orient_matrix_UB_32      -0.0559238000
_diffrn_orient_matrix_UB_33      -0.0178419000
_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  0.0343
_diffrn_reflns_av_unetI/netI     0.0470
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16717
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.834
_diffrn_reflns_theta_min         2.882
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.463
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.771
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.72a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.092
_exptl_crystal_description       block
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.175
_exptl_crystal_size_mid          0.128
_exptl_crystal_size_min          0.089
_refine_diff_density_max         0.473
_refine_diff_density_min         -0.286
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         8583
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0439
_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^)+(0.0669P)^2^+0.5674P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1163
_refine_ls_wR_factor_ref         0.1194
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7984
_reflns_number_total             8583
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc00909b2.cif
_cod_data_source_block           hasj180320a
_cod_depositor_comments
'Adding full bibliography for 1568860--1568864.cif.'
_cod_database_code               1568860
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         C94Ca2H160N4O2
_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. Restrained distances
 C43A-C44A \\sim C44-C43 \\sim C43A-C42A \\sim C43-C42 \\sim C42A_$1-C42A \\sim
C42_$1-C42
 with sigma of 0.02
 C44-C42 \\sim C44A-C42A
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C42A, C43A, C44A
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.003
4. Others
 Sof(C42A)=Sof(H42C)=Sof(H42D)=Sof(C43A)=Sof(H43C)=Sof(H43D)=Sof(C44A)=
 Sof(H44D)=Sof(H44E)=Sof(H44F)=1-FVAR(1)
 Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(C44)=Sof(H44A)=
 Sof(H44B)=Sof(H44C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C12(H12), C17(H17), C28(H28), C33(H33)
5.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C15(H15A,H15B), C18(H18A,H18B), C20(H20A,H20B), C29(H29A,
 H29B), C31(H31A,H31B), C34(H34A,H34B), C36(H36A,H36B), C38(H38A,H38B),
 C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B),
  C42A(H42C,H42D), C43A(H43C,H43D)
5.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C24(H24), C25(H25), C26(H26)
5.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C),
 C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C30(H30A,H30B,H30C), C32(H32A,H32B,
 H32C), C35(H35A,H35B,H35C), C37(H37A,H37B,H37C), C44(H44A,H44B,H44C),
 C44A(H44D,H44E,H44F)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              9441
_shelx_hkl_checksum              32570
_shelx_fab_checksum              20557
_olex2_date_sample_data_collection 2018-03-20
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.216
_oxdiff_exptl_absorpt_empirical_full_min 0.851